The method of processing organic substances, especially chloroorganics compounds containing effluent from epichlorohydrin production, and device for its implementation

 

(57) Abstract:

The invention relates to processing of organic substances, especially wastewater from the production of epichlorohydrin containing chloroorganics connections and drains coming or derived from the active reactor containing adsorbed organic halogen compounds in quantities of more than 10 mg/l, is subjected to at least two dichloride and/or dihydrochloride processing, the first stage effluent having a pH value of from 10 to 14, measured at room temperature, or set to this value serves as at least one subsequent reactor and/or provide through him, moreover, in the reactor establish or maintain the temperature of more than 75oC, a pressure of not less than 1 bar (abs.) and the aging period is not less than 0.5 h, and present in the effluent chloroorganics connection dechlorinate and/or dihydrochloride, on the second step of conducting at least one additional dahlerus and/or dihydrochloride processing mainly in the presence of hydrogen-containing gas or vodorodokislorodnye connection and/or in the presence of Catalytica acting substance, and then the treated effluent from the reactor or reactors to simplify the technological implementation, to reduce energy costs, limit the use of additional reagents. 2 C. and 20 C.p. F., 1 Il.

The invention concerns a method of processing organic substances, especially of wastewater from the production of epichlorohydrin containing chloroorganics connection, and epichlorohydrin, produced by the interaction dichloropropanol with at least one alkaline compound, preferably with a water solution containing calcium hydroxide, or suspension, and emitted from the reaction mixture by distillation, has an effluent quality of the product leaving the bottom of the column containing saturated and/or unsaturated aliphatic and/or alicyclic chloropalladite, chloroethene, Chlorophyta, chloroacetone, chloroacetamide and/or chlorocarbonate. The invention also applies to the installation for implementing this method.

Technical production epichlorohydrin (1-chloro-2,3-epoxy-propane) is based on the well-known appropriate method of dihydrochloride dichloropropanol with alkaline agents, predominantly aqueous solutions or suspensions of calcium hydroxide or sodium at elevated temperatures. Source material dichloropropanol polychaets the education of allylurea, chlorine and water.

Resulting from the above method epichlorohydrin stands out from the reaction mixture by distillation, mainly steam distillation. The product leaving the reactor synthesizer is an aqueous solution or suspension containing along with small amounts of the reaction product other organic, especially chloroorganics and inorganic compounds as by-products of synthesis, and not converted the original substance. This product in the effluent (when using calcium hydroxide as the alkaline agents in the synthesis of epichlorohydrin) usually contains the following substances: chlorinated cyclic or acyclic alkanes and alkenes, saturated and/or unsaturated aliphatic and/or alicyclic chloroethene, Chlorophyta, chloroacetone, chloroacetamide and/or chlorocarbonate, and along with other compounds contributing to the chemical oxygen demand of the effluent, especially glycerol and derivatives of glycerol, then calcium chloride, calciumcarbonat and perhaps excessively applied hydroxide of calcium.

Contained in the effluent chloroorganics connection --- the I as part of the organic halogen compounds (X = F, Cl, Br, I), adsorbed on activated carbon, and total adsorbed amount is set by the translation X = Cl.

Such effluents containing halogenated organic compounds represent a special problem for wastewater treatment, because the removal of these substances due to the high stability of the covalent bonds of carbon - halogen-free, especially when Halogens related SP, is technically expensive and therefore often unprofitable task.

Known measures for reducing chlorinated and other halogenated organic substances in the wastewater are physico-chemical and biotechnical technology.

Decomposition of halogenated organic compounds in biochemical purification stages of the treatment plant is associated with various problems. On the one hand, many of these compounds are not subject or a subject with great difficulty biodegradable by microorganisms. On the other hand, used in the effluent concentrations of substances that produce Oh should not be very high and, in addition, must have everywhere a constant value. In addition, in such installations, the large volume ASS="ptx2">

Therefore, in accordance with the prior art preferably provides methods of physico-chemical secretions halogenoalkanes compounds from wastewater, and these methods are used for preliminary or primary wastewater treatment (with subsequent biochemical processing).

Methods available for this purpose are, for example, treatment with activated carbon, as well as special methods of extraction. The disadvantage of these methods is the fact that they produce a secondary product, loaded with halogenated organic compounds (loaded activated carbon and/or extraction tool).

Repeatedly used measures of destruction halogenoalkanes compounds in the effluent are chemical and thermal methods. Here are the ways the so-called wet oxidation, which in oxidise atmosphere with high temperature and considerable pressure is the decomposition of halogenated organic compounds. These methods, although very effective, but are costly due to high energy consumption and expensive equipment.

To mitigate extreme physical conditions is their compounds, moreover, these substances can be incorporated by filing the appropriate reagents in dehalogenases system or are formed during the decay reaction as an intermediate product.

As substances having a high reactivity towards organically bound Halogens are used, for example, certain metals, metal hydrides or metalloelastase, separately or in combination with a strong organic base.

A disadvantage of the known physico-chemical methods for the degradation and/or destruction of halogenated organic compounds is their relatively high cost, which occurs especially when using expensive reagents and by installing oxidise or inert atmosphere, and the relatively high temperatures and pressures and the associated need to use expensive equipment. Moreover, in the economic balance of the known methods of dehalogenation and/or dehydrohalogenation halogenoalkanes compounds adversely affected by excessively long reaction time (often more than 10 hours) and often mediocre results of the decomposition.

Further known methods of processing waste is, partially dehalogenated and/or dehydrohalogenation by setting a certain temperature, pH and timing of exposure. According to the application DE-OS N 3620980 known expensive three-step method involving pre-treatment of wastewater by precipitation in the heat treatment step of hydrolysis, characterized by setting the pH to 11.5 using milk of lime and/or NaOH, the temperature is from 40 to 70oC and the aging period is from 1 to 3 o'clock

In accordance with another patent application WO N 92/05118 decomposition chlorolignin compounds is carried out at pH values from 6 to 11, a temperature of from 90 to 150oC, the excess pressure of from 70 to 475 kgf and aging period of 2-5 min, and the decomposition Oh to more than 60% is achieved mainly using other chemicals or due to the target mix of different effluents from the production of pulp bleaching (in this case, likely play a role in catalytic processes).

The suggested methods do not include references to their possible application for the treatment of wastewater generated during the synthesis of epichlorohydrin. Besides the above-mentioned methods of decomposition chlorolignin compounds in the effluent production is olego differences compositions of the effluents and the impossibility of transferring parameters on pH, temperature, pressure and period of exposure during processing, and thus, in particular, it is impossible to reach the percentage decomposition Oh more than 50%.

Evaluation of the aforementioned prior art economic method of removing halogenated organic compounds from industrial effluents should have the following characteristics: low technical costs when implementing the method, as simple as possible management response, low consumption of chemicals, as well as a high percentage decomposition Oh at low temperatures, pressures and short duration of exposure.

This method is especially for processing effluent from the synthesis of epichlorohydrin still could not be brought.

The invention therefore was to provide a way dichloride and/or dihydrochloride wastewater treatment, loaded chloroorganics substances, synthesis of epichlorohydrin characterized by simple technological management, low energy and hardware costs, and limited use of additional reagents, in order to solve the problems of wastewater known process for the synthesis of epichlorohydrin and thereby create a budget, the rd treatment technology for processing due to the process of precipitation.

There is an urgent need for at least partial removal chloroorganics compounds produced in the effluent of synthesizers epichlorohydrin, to perform environmental targets. This need is documented in the various patent applications in this specialized field, for example, in applications EP N 0247670, DE-OS N 3016667 and DE-OS N 3520019. Proposed options cover or expensive purification stages unwanted chloroorganics compounds or production process epichlorohydrin so modernized that allows you to minamiawaji education chloroorganics by-products. In any case, here we are talking about events that are associated with high costs and often leads only to a slight decrease in the organic chlorine compounds in the wastewater.

The subject of the invention is a method characterized in that the waste water leaving or withdrawn from the reaction vessel containing adsorbed organic halogen compounds (OOH) more than 10 mg/l, mainly 20 mg/l, are not less than two dichloride and/or dihydrochloride treatment during which the effluent is initially at the first stage in this pH value, served on at least one subsequent reactor and/or passed through the same reactor, and the reactor is installed and/or maintained at temperatures above the 75oC, mostly above 85oC, a pressure of not less than 1 bar (abs. ), mostly at least 2 bar (abs.) and duration of exposure at least 0.5 hours, mostly not less than 1 h, contained in the effluent chloroorganics connection partially dechlorinate and/or dihydrochloride and then at the second stage is carried out at least one subsequent degloria and/or dihydrochloride processing mainly in the presence of hydrogen-containing gas or releasing hydrogen compounds and/or in the presence of Catalytica acting substance, and then treated wastewater undergoes biological treatment using microorganisms.

The method according to this invention allows the cost-effective in large-scale production to dechlorinate and/or dehydrochlorinating chloroorganic compounds in the wastewater stream of synth epichlorohydrin with a high percentage of decomposition thus to solve in General, ecological and technical problems that have occurred so far with the disposal of these effluents.

In particular, it was found that by selecting the invention of the parameters of temperature, pressure and duration of exposure alkaline effluent from the synthesis of epichlorohydrin, which usually has a pH of from 11.5 to 12.5, the effluent may be subjected according to the invention and in this case without further increase in pH (due to the additive concerned basically existing connections) to process termolonkho dechlorination and/or dehydrochlorination in accordance with the first step of the method, and despite these relatively low pH is achieved surprisingly high percentage decomposition Oh.

Thanks to no less than two dichloride and/or dihydrochloride the treatment according to the invention at relatively low cost is almost complete decomposition Oh, at the first stage with reduced energy and maintenance costs, dash compounds, and then by a relatively small number of additional reagents is syrakousai dechlorination and/or dehydrochlorination, and decomposition Oh is mainly to such an extent that in the conclusion you get these effluents, which contain or even very small amounts of produce AOH components (mostly below 10 mg/l), or so reduced producing Oh substances that they can easily subjected to further biological treatment with the use of microorganisms for the final decomposition of residual organic compounds in the effluent.

Another advantage of the method according to the invention is the fact that for its implementation can be fundamentally used all used this prior art reactors, and does not require any special measures in respect of the execution of the walls of the reactor or existing installations, since in the method according to the invention, no problems with deposits or corrosion.

The unexpected fact was that despite the 'softened' terms invented in comparison with known methods for lower temperatures, pressures, and short and side-products of the synthesis of epichlorohydrin so, that option Oh effluent synthesis epichlorohydrin (according to a known method), which typically ranges from 25 - 45 mg/l, can be reduced to less than 100 mg/l, mainly to less than 5 mg l, and the remaining after dichloride and/or dihydrochloride processing, in this case, neutralized containing calcium chloride aqueous solution corresponded to the future of the legal provisions regarding the content AOH in industrial effluents.

Elimination of components containing Oh to more than 75%, mostly to more than 97% in the effluent synthesis epichlorohydrin is achieved due to the advantageous forms of embodiment of the invented method for the installation, pH, temperature, pressure and time of exposure, thereby providing a targeted regulation of the percentage of decay Oh.

Next, the wastewater is processed at the first processing stage, are in accordance with the first preferred form of execution of the pH from 11.5 to 12.5 (measured at room temperature) or are set to this value, and degloria or dihydrochloride processing contained in the effluent chloroorganics compounds is carried out in a reactor at a temperature of from 125 to 135oC, the pressure is now a form of execution of the invented method, the treated effluents are in the first process step the pH of 13 - 14 (measured at room temperature) or are set to this value and degloria and/or dihydrochloride processing contained in the effluent chlorinated organic compounds is carried out in a reactor at a temperature of from 125 to 135oC, a pressure of from 2.5 to 4, 0 bar (abs.) and the period of exposure effluents from 1 to 4 h

In accordance with another favorable form of execution of the invented method, the treated effluents are in the first process step the pH from 11.5 to 12.5 (measured at room temperature) or are set to this value, and degloria and/or dihydrochloride processing contained in the effluent chloroorganics compounds is carried out in a reactor at a temperature of from 175 to 185oC, a pressure of from 9.0 to 10.5 bar (abs.) and the aging period is from 1 to 8 hours

In accordance with another favorable form of execution of the invented method, the treated effluents are in the first process step the pH from 11.5 to 12.5 (measured at room temperature) or are set to this value, and degloria and/or dihydrochloride processing contained in the effluent chloroorganics compounds is carried out in a reactor at a temperature of from 85 to 90oC, a pressure of from 1.0 dlane invented method, the treated effluents are in the first process step the pH 11.5 - 12,5 (measured at room temperature) or are set to this value, and degloria and/or dihydrochloride processing contained in the effluent chloroorganics compounds is carried out in a reactor at a temperature of from 155 to 165oC, a pressure of from 5.0 to 7.4 bar (abs.) and the period of exposure of wastewater from 4 to 8 o'clock

In accordance with the invention it was found that even at relatively low temperatures and pressures, and pH values mostly in the range from 11.5 to 12.5 possible high level decomposition with the timing of exposure less than 10 hours, which represents an additional advantage of this method.

Further, as the opportune moment was found that as the aqueous solution containing calcium hydroxide, or suspension of the milk of lime may be used in the synthesis of epichlorohydrin with an excess of calcium hydroxide (relative to the calculated theoretical stoichiometric amount dichloropropanol required for complete reaction conversion), and the excess must be chosen so large that the treated effluent in the process generating these drains were installed at pH 11.5 to 12.5 (measured at collocini processing.

For installation under these conditions the pH (measured at room temperature) in accordance with the invention may be added an appropriate amount of alkaline or zameldowanie hydroxide, predominantly aqueous solution of sodium hydroxide and/or calcium.

Setting the pH value according to another advantageous form of execution of the invented method can also be undertaken through appropriate quantity of alkali carbonate and/or molochnokislogo carbonate, mainly due to an aqueous solution of sodium carbonate and/or hydrogencarbonate sodium.

Mainly termoselen treated wastewater flows to the subsequent reactor for further processing and there in the presence of hydrogen-containing gas or releasing hydrogen compounds and/or in the presence of a catalytically acting substance are then re-dichloride and/or dihydrochloride processing. The above re-degloria and/or dihydrochloride processing can be carried out in the reactor for thermoselect of treatment.

In a contrived way as the hydrogen-containing gas is mainly used high is artnum gas.

As a catalytically acting substance in the method according to the invention mainly uses a metal, metal alloy and/or inorganic and/or organic metallovedeniye or mixture of materials containing one or more data connections, and the catalytically active substance is applied with the addition of media, mainly the media containing alumina, for example, is applied to this carrier.

In accordance with another favorable Form of execution according to the invented method as Catalytica acting substance is applied compound containing palladium.

Because the effluent emerging from the synthesis reactor, especially when excessively applied lime milk as alkaline agents in the production of epichlorohydrin contain suspended solids, mainly undissolved calcium hydroxide, which can cause problems during processing, for example, due to the formation of blockages, it is advantageous to at least partially release the effluent in this case, before, during and/or after dichloride and/or dihydrochloride processing from suspended solids by the state by a chemical reaction, for example, by dissolution of the suspended calcium hydroxide by the addition of hydrochloric acid and/or by mechanical separation process such as filtration or sedimentation.

Implementation of the invented method can be carried out in continuous or intermittent mode, and is mainly used block reactors, consisting of at least three, preferably four, separate series or parallel connected reactors.

In connection with the above, in this case present in the wastewater, suspended solids, washing the treated wastewater stream is carried out mainly with the head part of the reactor and/or reactors descending down the stream, and the treated effluents are discharged from the bottom of the reactor. Washing effluent from the bottom of the reaction chamber upward flow could cause blockage of suspended solids.

For continuous implementation dichloride and/or dihydrochloride of treatment can also be used a hydraulic pipe or tubular reactor, in accordance with another favorable manner and is, preimushestvenno 8.5 m/s

The second step of the method according to the invention can be carried out in a reactor or reactors that have been used for the first stage of processing so that the pre-treated wastewater remains in the reactor or reactors at the end, for example, periodic regime carried out the first step and there by pumping and/or reagents for subsequent processing (through the appropriate supply device is further degloria and/or dihydrochloride processing. If termology treatment was carried out in continuous mode, the pre-treated wastewater after exiting the reactor or reactors back served on him or them to expose their subsequent dichloride and/or dihydrochloride processing in batch or continuous mode.

According to another form of execution of the invented method is processed at the first stage of the method, the effluent can be unloaded from the reactor or reactors and serve later on as a minimum, the following reactor for processing in accordance with the second step of the way.

For catalytic treatment in the second stage SP is predominantly a reactor with a fluidized bed.

Because the reactor for further processing wastewater can also cause problems with clogging due to suspended solids, the effluent prior to further dichloride and/or dihydrochloride processing are exempt from suspended solids mainly by a chemical reaction and/or mechanical method of separation, which, for example, may be similar to the above species.

Further beneficial factor can be cooled effluent prior to further processing and/or a change in pH value.

According to another form of execution invented by the method of processing wastewater in accordance with the first process step can be repeated at least once.

Heating the treated wastewater stream to a temperature treatment according to the invention can be carried out in conventional heating devices for heating can be used with electric or thermal energy, for example, accumulated in a hot pair.

To further improve the energy balance of the invented method enabling transfer of heat energy accumulated in the heated, processed and dreamie processing, moreover, there is a simultaneous cooling of the hot treated effluent stream. For this purpose the heat exchanger, through which the wastewater subjected to single or in this case, repeated treatment after discharge from the reactor and/or reactors for dechlorination and/or dehydrochlorination.

The heat transfer is mainly by direct transfer of heat by lowering the internal stress and condensation, i.e., discharge of hot, pressurized treated effluent especially with the formation of water vapor, which is supplied to a cold stream of wastewater that is not yet processed, with the transfer of the last of its heat through condensation.

According to another form of execution invented by way of direct transfer of heat is at least two, mostly three-stage.

During and/or after the heating phase invented method of treatment in the treated wastewater generation of free gases and/or vapours, in particular water vapor Laden with volatile organic compounds. These gases and/or vapors in accordance with the becoming is a process i.e., in the synthesis reactor of epichlorohydrin.

Mainly on the basis of the invented method are processed wastewater synthesis epichlorohydrin with a total content of soluble organic substances more than 0.15 g/HP

Further processed according to the invented method dechlorination and/or dehydrochlorination drains mainly after cooling, subjected to further purification, mainly biological treatment using microorganisms. Thanks to the pre-reduction value AOH in accordance with the invented method in the effluent synthesis epichlorohydrin becomes possible subsequent biochemical and/or biological decomposition of the remaining organic compounds by the bacteria, and due to microbiological decomposition at the same time also decreases the value of GSB (chemical oxygen demand) of the effluent that resulting from destruction soluble in the effluent organic compounds (occurring as derivative products of the dechlorination process and/or dehydrochlorination and as by-products from the synthesis of epichlorohydrin) due to the activity of the metabolism of microorganisms.

Sullenger, can also directly be fed to the biological treatment.

Biological treatment may be performed under aerobic or neuronal mode.

Before biological treatment in this case can be taken corresponding change in pH for the availability of wastewater microbiological processing.

The invention relates further installation for processing by dechlorination and/or dehydrochlorination of wastewater from the production of epichlorohydrin containing chloroorganics connection, and carrying out processing is carried out mainly by one or more technological claims.

A significant characteristic of the installation according to the invention must be the fact that the plant can be used, in particular, as an industrial unit, allowing optimisation cheap holding dichloride and/or dihydrochloride of treatment, and in the installation according to the invention should be used mostly standard equipment.

It was determined that this setup (see drawing ) differs in that it contains at least one precipitator (2), at least one heating device (9), not less onnee three series or parallel connected reactors (4, 5, 6). The above sign indicates that, in particular, when using at least three, and especially four, reactors for dechlorination and/or dehydrochlorination in continuous or periodic mode is achieved by the optimisation method is relatively lower values AOH, as well as manufacturing and maintenance costs.

According to a preferred form of execution of the installation according to the invention as precipitator (2) is used sedimentation precipitator, in which the suspended solids is at least partially removed from drains under the action of gravity, since the settling of solids in the heat exchanger and/or the reactor or reactors leads to blockage and/or from in the above-mentioned apparatus, as a result you may experience production shutdowns for cleaning work to remove sediment solids.

As sedimentation precipitator used normal precipitation apparatus, and they can be used both in intermittent and continuous mode.

Precipitation apparatus should preferably be equipped with fungal mechanism located on the middle VTI rotation fungal mechanism is less than 2.5.min, mostly 1.5 on. /min to maintain the movement of wastewater to prevent deposition segmentierung solids in the precipitator.

As reactors can be used in a conventional reaction vessel and/or columns, and they should also be equipped with a mixing device for mixing wastewater. The walls of the reactor are mostly composed of non-alloy steel, because wastewater treatment according to the invention does not cause corrosion problems.

Precipitator (2) and/or reactor or each individual reactor (4, 5, 6) are predominantly conical shape, with each of the reaction vessels and/or precipitation capacity are, in particular, the conical lower part.

In order to prevent clogging and/or the formation of deposits in the precipitator (2) and/or reactor or in each individual reactor (4, 5, 6) in accordance with another preferred form of execution of the installation according to the invention each of the above types of apparatus has a conical angle less than 120oC, mostly 90o.

To obtain favorable hydraulic characteristics in accordance with another preferred form of execution to ustanovlenytakie thus, to each of the above types of equipment the ratio between the total height and diameter of the reaction or precipitation capacity was more than 2, preferably of 2.5.

If the choice of dimensions is that of the relationship between the cylindrical height and diameter precipitator (2) and/or reactor or each individual reactor (4, 5, 6), then this ratio should be in each case more than 1.4, preferably of 1.7.

Preliminary and/or primary heating the treated effluent to a temperature dechlorination and/or dehydrochlorination according to the invention is carried out in conventional heating devices.

After the first loop can be made direct or indirect heating of the subsequent incoming raw wastewater hot output stream is already treated effluent and at least part of the accumulated heat is transferred to the cooler, raw sewage flow, due to which there is a simultaneous cooling leaving the reaction zone, the treated wastewater.

For this purpose one or more heat exchangers, which may be of conventional type and exploitati in the reactor (7) for holding dichloride and/or dihydrochloride processing according to the second process stage. Mainly it uses a reactor with a fixed catalyst or fluidized bed, mostly, a reactor with a fluidized bed.

According to another preferred form of execution of the installation according to the invention the reactor or each individual reactor (4, 5, 6) each equipped with at least one connection for supplying a hydrogen-containing gas or vodorodovozdushnoi connection and/or Catalytica acting substance. To download effluent hydrogen-containing gas can, for example, be used as the at least one scrubber or at least one injection system.

It is possible to install for technical implementation of the method according to the invention and a schematic representation of the preferential process control in the form of a flow chart shown in the drawing.

The drawing refers to the continuous mode. From the synthesis reactor epichlorohydrin (drawing not shown) by means of a pump 1 waste water to be processed through the input device A are fed to the sedimentation precipitator 2, in which the effluent is at least partially freed from the solids. By means of the second pump 3 through the bypass device C assessa unloading purified stream sedimentation precipitator at the top of the sump.

The wastewater is then released (if already held the first processing cycle and is available in hot, treated wastewater flows) to the heat exchanger 8 where it is warm already treated effluent is transferred to raw incoming stream in such a way that is energy efficient heating wastewater. Hot wastewater stream that acts as an energy source, passes through a feed device D on the heat exchanger and after the energy transfer, by means of which the cooling of the treated wastewater flows through the outlet device H is diverted from the heat exchanger and is supplied to the discharge device E for further processing and/or further use of wastewater.

Further heating of the raw wastewater flows to the final temperature dechlorination and/or dehydrochlorination is carried out in the heating device 9, which is connected by a pipe I with the heat exchanger. As heating medium is used, for example, hot steam, which is supplied to the heating device through the supply line J.

Heated waste water through the supply line G is then supplied in three sequence is s water arrives at the head of each of the reaction vessels and discharged through the discharge outlet in the lower part of the respective reactor. The reactor is thread-safe. Sewage remains in the reactor in accordance with the period of exposure and at the end of the processing time are fed to the precipitator solids 10, in which the effluent by adding hydrochloric acid using pump 12 is set to such a value of pH at which the suspended calcium hydroxide is at least partially converted into solution. Remaining after solids are separated from the effluent and removed through line L of the precipitator solids. Supply of hydrochloric acid in the scrubber 11 through the pipe N. the Mixture of effluent with hydrogen supplied through the pipe O into the reactor 7, which is mainly performed as installing a fluidized bed, and it drains undergo additional dichloride and/or dihydrochloride processing. Through the outlet pipe D drains at the end of processing are fed to the heat exchanger 8.

Before and/or after the filing of the treated effluent from the heat exchanger can be taken further separation of suspended solids from the treated wastewater. It occurs mainly in sedimentation precipitator.

During the heating and during the processing of the flow is borrowed F disposed in the synthesis reactor of epichlorohydrin.

Next is the drain pipe C to sedimentation sump precipitator 2 can be used to set the pH of the treated effluent stream E to such an extent that the effluent could then be subjected to microbiological processing.

Underlying the following examples of performance experiments are required to explain the invention without restricting it to these examples.

Example 1. 1 liter of wastewater from the production of epichlorohydrin content AOH about 35 mg/l and a pH value of 12 (measured at room temperature) was subjected in accordance with the invention thermoselect dichloride and/or dihydrochloride processing in the reactor for 3 hours at a temperature of 85oC and a pressure of 1 bar (abs.). Due to this content AOH could be reduced by about 30%.

Then by adding hydrochloric acid in the effluent was set to pH 10, and the residual solids were separated by sedimentation. Then the effluent was treated in the fluidized bed for 1 h at room temperature in the presence of hydrogen and containing a palladium catalyst. The content AOH could be reduced by 83%.

Example 2. 1 l of wastewater from production epichlo in accordance with the invention thermoselect dichloride and/or dihydrochloride processing in the reactor for 3 hours at a temperature of 130oC and a pressure of 2.5 bar (abs.). Due to this content AOH could be reduced by about 66%.

Then by adding hydrochloric acid in the effluent was set to pH 10, and the residual solids were removed by sedimentation. Then the effluent was treated in the fluidized bed for 1 h at room temperature in the presence of hydrogen and containing a palladium catalyst. The content AOH could be reduced by 91%.

Example 3. 1 l of wastewater from the production of epichlorohydrin was termoselen processed analogously to example 2, and then by adding hydrochloric acid was set to a pH value of 10.5, cooled and subjected to aerobic biological treatment at 20oC and the average duration of exposure 10 o'clock by this measure the content AOH in the effluent could be reduced by about 75%, and the value of the CSB is at about 85%.

Example 4. 1 l of wastewater from the production of epichlorohydrin was termoselen and Catalytica processed analogously to example 2, and then subjected to aerobic biological treatment at a temperature of 26oC and the average duration of exposure 7 hours Due to this the value of the CSB was reduced by more than 85%.

1. The method of processing organic substances, the sedge in the reactor, characterized in that the allocated or discharge wastewater containing adsorbed organic halogen compounds in quantities of more than 10 mg/l and pH 10 to 14, measured at room temperature, or set at this value of pH, served in at least one subsequent reactor and/or leave on the ground when handling or exposure in the reactor for 0.5 h at a temperature above the 75oC, pressure of not less than 1 ATM (abs.) followed declaraciones and/or dehydrochlorination processing in the presence of hydrogen-containing gas or releasing hydrogen compounds and/or in the presence of Catalytica acting substance, after which the treated wastewater is unloaded from the reactor or reactors and/or subjected to iobrabotki using microorganisms.

2. The method according to p. 1, characterized in that the effluent with a pH value of 11 to 14, measured at room temperature, subjected to heat treatment at a temperature of 85 - 185oC, at a pressure of 2 to 10.5 bar (abs.) for 1 to 8 h, followed by declaratia and/or dihydrochloride in the presence of high-purity hydrogen at the same time as Catalytica current substance use metal, metal alloy and/or nieorganiczne, with the addition of the substance carrier.

3. The method according to p. 2, characterized in that the mixture material contains a compound containing palladium.

4. The method according to PP.2 and 3, characterized in that the used substance is a carrier containing alumina.

5. The method according to PP.1 to 4, characterized in that the treated effluents contain more than 0.15 g/l of soluble organic materials.

6. The method according to PP.1 to 5, characterized in that deklaraciu and/or dehydrochlorination produced in the reactor unit consisting of at least three reactors, the reactor used hydraulic pipe or tubular reactor installation in a hydraulic pipe or tubular reactor flow rate of more than 4 m/s

7. The method according to p. 6, characterized in that the reactor unit consists of four reactors.

8. The method according to PP.6 and 7, characterized in that the hydraulic tube or pipe reactor establish the flow velocity of 8.5 m/s

9. The method according to one or more of the paragraphs.1 to 8, characterized in that the effluent before, during and/or after dechlorination and/or dihydrochloride at least partially released from the suspension of solids.

10. The method according to p. 9, wherein retrieving the BU separation.

11. The device for carrying out processing chloroorganics compounds containing effluents from the production of epichlorohydrin, including the reactor, characterized in that it has at least one precipitator, at least one heating element, at least one heat exchanger and at least one reactor, the precipitator and/or the reactor or each reactor has a tapered shape.

12. The device according to p. 11, characterized in that it has a reactor block with four in series and connected in parallel reactors.

13. The device according to PP.11 and 12, characterized in that use precipitator sedimentation type.

14. The device according to PP.11 to 13, characterized in that the ratio between the total height and diameter of the precipitator and/or the reactor or each individual reactor in each case greater than 2.0, the ratio of cylinder height and diameter of the precipitator and/or the reactor or each individual reactor in each case, more than 1.4 and the angle of the cone precipitator and/or the reactor or each individual reactor in each case less than 1200o.

15. The device according to p. 14, characterized in that the ratio between the total height and diameter of the precipitator and/or reactored cylindrical height and diameter of the precipitator and/or the reactor or each individual reactor 1,7.

17. The device according to PP.14 to 16, characterized in that the cone angle of the precipitator and/or the reactor or each individual reactor 90o.

18. The device according to PP. 13 to 17, characterized in that the sedimentation precipitator equipped Gribkova mechanism, develop a rotation speed less than 2.5.minutes

19. The device under item 18, characterized in that grabowy mechanism has a maximum speed of 1.5 rpm./minutes

20. The device according to PP.14 to 19, characterized in that the reactor is made in the form of a reactor with a fixed catalyst or fluidized bed and serves to conduct dichloride and/or dihydrochloride processing in accordance with the second process step.

21. The device according to p. 20, characterized in that the reactor is made in the form of a reactor with a fluidized bed.

22. The device according to PP.18 to 21, characterized in that the reactor or each reactor comprises at least one inlet pipe for hydrogen gas or bogoroditsye connection and/or Catalytica acting substance.

 

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