Method for treatment of phenol from impurities

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to manufacturing phenol by cumene method, in particular, to a step for treatment of final product and preparing phenol of high purity degree. Method for treatment of crude phenol is carried out for two steps. At the first step method involves oxidation of acetol, aldehydes and α-methylstyrene with air oxygen in phenol medium by using a heterogeneous catalyst comprising metals with transient valence. At the second step method involves condensation of oxidation products and non-oxidized products by using a heterogeneous acid catalyst. Separation of compounds in the process of phenol treatment is carried out on the final step of isolation of the commercial product by distillation method. At the first stage metal compounds of by-side subgroups 1 and 6 and metals of 8 group of Periodic system on neutral or acid carrier are used as a catalyst preferably. At the second step alumosilicate contacts based on zeolites of type "X" or "Y", or other zeolites comprising or not comprising promoting and modifying additives are used as a catalyst. Invention provides the high degree of purification of phenol from impurities and the improvement of economy indices of the process.

EFFECT: improved method for phenol treatment.

12 cl, 5 ex

 

The invention relates to the production of phenol Kukolnik method, in particular to a method of purification of phenol from impurities (and unsaturated carbonylic impurities), with the aim of obtaining phenol of high purity, meeting the highest requirements of the consumer.

The main industrial method for the production of phenol now became komorny method including chemical oxidation steps isopropyl-benzene (cumene) cumylhydroperoxide (CCP) and its subsequent decay in the presence of acid catalyst to phenol and acetone. Chemical characteristics of the process of production of phenol Kukolnik way to determine the composition of the resulting adverse chemical compounds that fall into marketable products as impurities. The main impurities deteriorating consumer properties of the materials obtained during the subsequent processing of the phenol include alkylaromatic, and unsaturated carbonyl compounds, in particular α-methylsterol (AMC), the oxide mesityl (ACM), Foron, 2-methylbenzofuran (ICF), oksuzyan (acetal), Cresols, etc. are Some of the possible ways of formation and subsequent directions of transformation of impurities represented by the following reactions:

The phenol used in the manufacture of medical preparations and some floor the dimensional materials, there are increased requirements on the content of impurities, which must not exceed the value of 0.0100 wt.% In this case, it is necessary to use special methods of purification of phenol.

Existing methods for removal of phenol from impurities based on the use of physical and chemical methods. Physical methods of separation of undesirable compounds are reduced to the use of distillation, azeotropic distillation and extraction [United States patents US 2744144 US, US 4532012, US 3405038, US 4504364 037/76].

Disadvantages common in industrial practice physical treatment of phenol are very high energy costs and increased sensitivity to the magnitude of the volumetric load on raw: the increase in the rate of feed of raw material against the project is accompanied by degradation of phenol.

List of used chemical methods for removal of phenol from impurities sufficiently broad and takes into account the chemical nature of the compounds, pollutants phenol. Basic common chemical methods of removing impurities based on the use of the above reactions with subsequent distillation separation from phenol formed of the condensation products. As catalysts usually used homogeneous acid catalysts [US patent US 3810946], as well as alkaline catalysts [US patent US 3335070].

From the local the way in which, along with the processing of phenol alkali to bring the pH to values 7-9, carry out the oxidation by air oxygen [European patent EP 1188477, U.S. patent US 3862244].

Some of the known methods for removing impurities focused on specific chemical compounds that can impair one or the other most important quality indicator of phenol.

Examples of this approach can serve as ways to remove acetal. Acetal and formed from him ICF degrade the color produced commercial phenol and plastics based on it. Because the indicator color is very important to ensure the use of special methods, different approaches to problem solving.

Most traditional methods are focused on the removal of impurities of acetol and ICF phenolic stream, where they accumulate in the rectification process of decomposition products of the CCP. This is done using physical methods mentioned water-extractive distillation and extraction, as well as some chemical methods. Known, in particular, the method of removing acetal of phenol, which consists in turning it into a heavy nitrogenous compounds by adding high molecular weight amines [United States patents US 3322651, US 3692845].

The disadvantage of this method is the high cost of amines, as well as problems with processors is some waste nitrogen compounds, which cannot be done without a negative impact on the environment.

A fundamentally different approach to measure the color of the phenol is a method based on prevention education ICF in the process of rectification by preceding this stage extraction acetal of the decomposition products of the CCP circulating water-salt solution [U.S. patent US 6066767]. In the specified method at pH>7 the transformation of the extracted acetal and aldehydes in deep condensation is carried out in a separately installable reactor at temperatures up to 130°C.

This method is effective for removing acetal and, accordingly, ICF, but requires the use of multi-stage extraction is capital and energy intensive.

The method according to U.S. patent 6573408 borrows the approach described above to remove acetol, but it reduces the number of stages of extraction to the one at pH 3-6, and high temperature processing of water-salt solution up to 300°C.

The introduction of these changes, however, only reduces the degree of extraction of acetol of the decomposition products of the CCP and so increases the energy costs in the process that the method becomes economically unjustified.

Significant reduction in capital-intensive processes based on the use of methods is straccia and subsequent transformation of acetal in water-salt solution, allows you to achieve the described method of oxidizing (air) turning acetal [Refining and petrochemicals. 2000, vyp. C. 507-510]. Oxidation of acetal in the presence of an alkaline catalyst flows with speed, ˜10 times higher than the rate of condensation reactions that can proportionally reduce the size of the reactor.

The disadvantage of having to use a multistage extraction for complete extraction of acetol, remains.

There is also a way to remove acetal, unsuccessfully combining known methods of extraction of acetol water-salt solution [U.S. patent US 6066767] and using the oxidation method of making it in this environment [Refining and petrochemicals. 2000, vyp. C. 507-510], where the oxidant at pH 3-6 proposed to use hydrogen peroxide, salts thereof, and alkali metal permanganates [US patent US 6576798]. It is known that the extraction in a water-salt solution along with acatalog pass phenol and acetone, and their concentration in ˜10 times the content of acerola. It is on the oxidation of these target products of the process is spent 96-97% Rel. fed to the reactor inorganic oxidant, leading to huge consumption of expensive chemicals and unnecessary economic costs.

The most common in the industry the industry is a method of purification of phenol from impurities on heterogeneous acid catalysts, which is often used sulfonic cation. This method has the obvious advantage over methods based on the use of directly acids or alkalis that its use does not generate wastewater. However, the use of sulfonic cation as catalysts for purification is not without flaws. These catalysts are polymeric materials having a low mechanical strength and thermal stability and are prone to swelling and cracking during operation. Selfactivity the catalysts for purification of phenol have a limited lifespan, not regenerated and after unloading processed by incineration in a special oven.

The closest analogue is the method of purification of phenol from impurities (carbonyl compounds and unsaturated compounds), including the contacting of the phenol with the zeolite catalyst is a mineral catalysts, in particular, promoted aluminosilicates with a pore diameter of more than 4 angstroms at atmospheric pressure or pressure, which ensures the presence of phenol in the liquid state and at a temperature of from 120°, 250°C. These catalysts do not have temperature limitations for use in the present process, mechanically strong enough and can be regenerated to what Sloboda air with the return of original properties. Unfortunately zeolite catalysts are not universal in relation to the processing of the entire spectrum of impurities present in the phenol. In particular, in the presence of zeolite catalysts effectively runs the purification of phenol from ACM and AMC, whereas MBF not converted. Moreover, while acetal present as impurities in the phenol, in the conditions of zeolite catalysis is fully converted, its disappearance is accompanied by the appearance of the ICF, which is the product of the interaction of acetol with phenol.

The present invention is to develop an effective method of purification of phenol, which eliminates the above disadvantages.

The task is solved by the proposed method for purification of phenol from impurities, in which the first stage in the environment phenol raw conducting the oxidation of the impurities oxygen using a heterogeneous catalyst containing a metal of variable valence, and the second stage are condensation products of oxidation and not oxidized impurities using heterogeneous acid catalyst, followed by separation of commodity phenol by distillation.

Preferably the oxidation of the impurities oxygen and condensation of oxidation products and not oxidized impurities carried out in a single reactor using one or not is how many types of heterogeneous catalysts, containing metals of variable valence and having acid properties. The temperature in the reactor or reactors purification from impurities should be maintained in the range of 50-250°With, it is most preferable to maintain the temperature in the reactor in the range of 80-210°C. as the catalyst in the first stage are used compounds of the metals of auxiliary groups 1 and 6 groups, and metals of the 8th group of the Periodic table in a neutral or acidic media. As the catalyst in the second stage, it is preferable to use alumina contacts on the basis of zeolites of type "X"or "Y"or other zeolites, containing or not containing the promoting and modifying additives, and catalysts in the second stage may have a preferred size of the input window is greater than 6 angstroms or be a cation type KU-2, KU-23, Amberlyst, Amberlite, Lewatit and others.

Preferably, in the reactor as the catalyst of the second stage to use a combination of aluminosilicate contacts on the basis of zeolites of type "X"or "Y"or other zeolites and ion exchangers type KU-2, KU-23, Amberlyst, Amberlite, Lewatit and others.

Preferably as a carrier for catalyst for the first stage of the use of carbon sorbents, neutral form of aluminum oxide and its salts, and also salts of metals of main group 2 group Intermittent the second table, moreover, the concentration of the active metal on the carrier can be 1-60 wt.% in the calculation of the oxide of the active metal.

The air in the reactor can range 0.1-80 h-1most preferably, 1-40 h-1in the calculation of the catalyst.

The proposed method is that the process of purification of phenol from impurities is carried out in two stages on the catalysts of various types and at various operating parameters. At the first stage of filtration is the oxidative conversion of acetol and partial conversion of the impurities AMC, cumene and DMPC in the discharge from phenol by distillation products. In the second stage completes the purification of phenol from these and other impurities on heterogeneous acid catalysts, carried out before the final distillation of phenol raw obtaining pure commodity product.

The first stage is almost complete conversion of acetol environment phenol raw and partial conversion of other impurities. However, due to the use of a special catalyst and the process mode, the oxidative conversion of acetol flows under conditions precluding the formation of ICF and prevent the oxidation of phenol. No acetol in the product obtained in the first stage of purification, allows you to complete the purification of phenol-raw aluminosilicate catalysts or sulfonic cation exchanger is without fear to achieve concentrations of ICF, which may have a negative impact on the quality of the commodity phenol.

As catalysts for the first stage of purification of phenol using metal compounds, preferably oxides) side of subgroups 1 (preferably copper) and 6 groups (preferably molybdenum), and metals of the 8th group (preferably Nickel and cobalt) of the Periodic table on a neutral carrier, having a minimum number of proton and aprotic acid sites. As carriers it is best to use coal, inactive, aluminum hydroxide, and magnesium oxide, as well as carbonates, sulphates and phosphates of metals of the 2nd and 3rd groups of the Periodic table. Most preferably used as the carrier specially prepared calcium phosphate. This media and catalysts based on it have a high stability in the conditions of the process of purification of phenol. In addition, the catalyst is partially lost activity during a long operation, unlike sulfonic cation, may be subjected to steam or an oxidizing regeneration to restore the original properties.

Method steam treatment is applied for purification catalyst from phenol sorbed during operation, with subsequent processing of the received the phenol-contaminated water at the existing phenol is different plants sites definalely. Exhaust and steamed catalyst does not differ from natural mineral Apatite, does not require special disposal methods, because there is no danger to the environment and, if necessary, can be processed to extract the active metal-promoter.

As catalysts in the second stage of purification of phenol using medium and broad porous aluminosilicates, promoted or without supplementation of certain promoters and modifiers and formed with one or another binder. It is preferable to use catalysts based on zeolites X and Y zeolites index FAU on the classification of the International Zeolite Association). For the purification of phenol in the second stage can be used as the sulfonic cation of different brands and directly sulphuric acid.

The volumetric feed rate to the first and second stage of filtration is determined by the concentration of impurities in the phenol, but usually varies in the range of 0.2 to 3 h-1. The optimal value of the volumetric feed rate of the raw material on the first and second stages of the purification of phenol may vary, in the continuous process is ensured by the selection of the volume of the reactor.

Air speed 1-40 h-1is only the first stage of purification of phenol, when the first reactor and the second stage separated. Correctly selected mode is rosedene process allows the oxidation of the impurities, in particular, acetal with a speed exceeding the speed of their interaction with phenol. This allows you to completely eliminate the formation of the ICF and to prevent associated with its negative consequences.

Complete metamorphosis of acetol on the first stage of purification of phenol greatly simplifies the task of purification of phenol on the second stage at which to remove residual concentrations and unsaturated carbonylic compounds suitable wide range of zeolite catalysts and sulfonic cation.

Below are examples that illustrate the proposed method, but not limiting of the claims of the applicant.

Example 1

18 g of finely pulverized in a mortar of calcium molybdate was mixed in a kneading machine with 160 g of powdered disubstituted calcium phosphate, was added 50 ml of water and was plastifitsirovanie for 1 hour. The resulting mass was molded by using an extruder, dried at a temperature of 120°C for 12 h and was progulivali 3 hours at a temperature of 350°C.

The prepared catalyst was placed in a flow reactor, heated with an electric furnace. A second similar reactor, connected in series with the first, was loaded zeolite catalyst "Zakar - C10".

The raw material used phenol containing impurities and unsaturated carbonylic compounds, pepper and concentrations are given in Table 1.

Source raw materials from the heated tank dosing pump is supplied to the mixer for mixing with the incoming into the reactor with air, and further enriched air mixture is fed to the first reactor. Emerging from the reactor product stream is passed to the separator, in which the separation of air and liquid phenol was entered in the second reactor. The temperature in the reactors of the cascade was supported by electrical heating. The reaction product after cooling was subjected to GC analysis to determine the content of impurities. The composition of the feedstock and operating process parameters, including temperature reactors, the feed rate and air, as well as the content of impurities in the resulting product are shown in Table 1.

Example 2 (for comparison)

Purification of phenol was carried out as in example 1 with the difference that the first reactor was turned off, and the raw material was applied directly to the second reactor. The content of impurities in the resulting product for this case are shown in Table 1.

Example 3

The catalyst was prepared analogously to example 1 with the difference that calcium phosphate was replaced with an equal amount of magnesium oxide. Purification of phenol was carried out as in example 1 with the difference that in the second reactor was loaded sulfonation KU-2-cs. The composition of the feedstock and operating parameters of the process, including the temperature of the reactor, near the al raw material supply and air, as well as the content of impurities in the resulting product are shown in Table 1.

Example 4

To a solution obtained by mixing 497 g of Nickel nitrate [Ni(NO3)2×6H2O] in 1200 ml of water and 379 g of chromium nitrate [Cr(NO3)3×9H2O] in 1000 ml of water, was added with stirring for 1 hour a solution of 305 g of ammonium carbonate [(NH4)2CO3] in 2000 ml of distilled water. The precipitation was filtered, washed with water, dried at 110-120°10 hours and progulivali at 300°3 hours. To thoroughly pounded in a mortar and the powder was added 8 g of powdered graphite were mixed and formed into tablets on a laboratory press.

The catalyst was placed in the first reactor and conducted clearing phenol analogously to example 3 under the changed conditions. The composition of the feedstock and operating process parameters, including temperature reactors, the feed rate and air, as well as the content of impurities in the resulting product are shown in Table 1.

Example 5

To a solution obtained by mixing 302 g of copper nitrate [Cu(NO3)2×3H2O], of 69.2 g of chromium nitrate [Cr(NO3)3×9H2O], and 10.5 g of barium nitrate [BA(NO3)2] and 228 g of zinc nitrate [Zn(NO3)2×6H2O] in 1500 ml of distilled water, was added a solution of 300 g of ammonium carbonate [(NH4)2CO3] in 200 ml of distilled water. The precipitation was filtered, washed with water, dried at 110-120°10 hours and progulivali at 300°3 hours. To thoroughly pounded in a mortar and the powder was added 8 g of powdered graphite were mixed and formed into tablets on a laboratory press.

The catalyst was placed in the first reactor and conducted clearing phenol analogously to example 3 under the changed conditions. The composition of the feedstock and operating process parameters, including temperature reactors, the feed rate and air, as well as the content of impurities in the resulting product are shown in Table 1.

Table 1
Number example12345
The number of reactorraw materialsIIIraw materialsIIIraw materialsIIIraw materialsIIIraw materialsIII
Flow, ml/h:
raw materials12121277121277
air60--120-60-120-
The volumetric rate
raw, 1/h111111111
The volumetric rateȊ
air, 1/h510510
Temperature, °12020020018090170909090
Content
products, parts on
million:
ACM110100011001109001109001101100
AMC390700390012010001201100120500
DMFC18000180050300504005000
the cumene1050100100 010001050
acetal4800048004601004804001080400
2-ICF90707090570706040909050908060

1. The method of purification of phenol from impurities, in which the first stage of conducting an oxidation reaction of the impurities with oxygen using a heterogeneous catalyst containing the oxides and(or) salts of metals of variable valency, and the second stage are condensation products of oxidized and non-oxidized impurities using heterogeneous acid catalyst, followed by separation of the phenol by distillation.

2. The method according to claim 1, in which the oxidation of the impurities oxygen and condensation and oxidation products of oxygenated products is carried out in a single reactor using one or more types of heterogeneous catalysts containing metals alternating the valence and having acid properties.

3. The method according to claim 2, in which the temperature in the reactor or reactors support from impurities in the range of 50-250°C.

4. The method according to claim 2, in which the temperature in the reactor from impurities is supported in the interval 80-210°C.

5. The method according to claim 1, wherein as the catalyst in the first stage are used compounds of the metals of auxiliary groups 1 and 6 groups, and metals of the 8th group of the Periodic table in a neutral or acidic media.

6. The method according to claim 1, wherein as the catalyst in the second stage uses aluminosilicate contacts on the basis of zeolites of type "X"or "Y"or other zeolites, containing or not containing the promoting and modifiers.

7. The method according to claim 1, wherein the catalysts in the second stage have the preferred size of the input window is greater than 6 angstroms.

8. The method according to claim 1, wherein as the catalyst in the second stage using the cation type "RL-2", "KU-23", "Amberlyst", "Amberlite", "Lewatit" and others.

9. The method according to claim 2, in which the reactor as catalysts use a combination of aluminosilicate contacts on the basis of zeolites of type "X"or "Y" or other zeolites and ion exchangers type "RL-2", "KU-23", "Amberlyst", "Amberlite", "Lewatit" and others.

10. The method according to claim 1, in which as a carrier for the catalyst of the first stage carbon sorbents, neutral form of aluminum oxide and from whom, and as well as salts of metals of main group 2 group of the Periodic table.

11. The method according to claim 5, in which the concentration of the active metal on the carrier is 1-60 wt.% in the calculation of the oxide of the active metal.

12. The method according to claims 1 and 2, in which the air supply to the reactor is 0.1-40 h-1in the calculation of the catalyst.



 

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