Method of obtaining calcium stearate

FIELD: chemistry.

SUBSTANCE: invention relates to improved method of obtaining calcium stearate by interaction of stearic acid and calcium hydroxide with heating and intensive mixing, further filtration and drying of sediment. Interaction of stearic acid and calcium hydroxide is performed in water medium, with emulsion being heated to 58-65°C, being brought into state of stable emulsion, kept at said temperature for 20-40 minutes until solution pH is 8.0-9.0, with further thermal processing for aggregation of particles with constant stirring and increase of temperature to 70-85°C, and exposure for 10-15 minutes to solution pH 7.5-9.0; after which water is poured in and mixing and filtration are carried out.

EFFECT: method makes it possible to simplify technological process, reduce calcium hydroxide consumption.

1 tbl,1 ex

 

The technical field to which the invention relates.

The invention relates to petrochemical synthesis, in particular, to a method for producing calcium stearate, and can be used as a thermo stabilizer in the production of polyvinyl chloride resins (PVC) in the processing of plastics, in the manufacture of artificial leather and linoleum, as well as in the production of vitamin tablets, medicines and scientific purposes.

The level of technology

A method of obtaining calcium stearate exchange reaction of decomposition of sodium stearate with calcium chloride (see Beggarwood. Chemistry and technology of stabilizers in polymeric materials. M., "Chemistry", 1981, p.150).

The disadvantage of this method is the necessity of washing stearate calcium from chlorine ions, which leads to the formation of large quantities of wash water.

A method of obtaining calcium stearate interaction of stearic acid and oxide or hydroxide of calcium when equimole the ratio of reagents and vigorous stirring, the process is carried out in the solid phase at atmospheric pressure and a temperature of 18 -25°C in the presence of zeolite type Sakh in the amount of 6,7-16 wt.% (see U.S. Pat. RU # 2259993, CL SS 51/41, SS 53/126, publ. 10.09.2005,).

The disadvantage of this method is the complexity of the technological process, high energy intensity.

p> The closest in technical essence and the achieved positive effect and adopted by the authors for the prototype is the way to obtain calcium stearate, the essence of which consists in the following. Stearic acid is dissolved at 70-75°C in 4-6-fold excess relative to the weight of stearic acid in aqueous-alcoholic solution at a volume ratio of alcohol: water(1,5...0,5):(0,5... 1,5) accordingly, sportowego solution using the solutions of C1-C4 alcohols, the time of dissolution 30-40 minutes, then the mixture is subjected to interaction with 18-25%aqueous solution of calcium hydroxide, with the molar ratio of stearic acid and an aqueous solution of calcium hydroxide 2:(1,3...1.5), reaction time of 2 hours, the finished product with an acid number of 2 mg KOH/g is filtered off, washed with water and dried with hot air at 80 to 90°C, the product yield is 99,2% (see U.S. Pat. RU # 2124495, CL SS 51/41, SS 53/126, publ. 10.01.1999 year).

The disadvantage of this method is the complexity of the technological process, deadweight loss sportowego solution and process in excess calcium hydroxide lead to appreciation of the process.

Disclosure of inventions

The task of the invention is to develop a method of obtaining calcium stearate, with the simplification process is ECCA, the cost.

The technical result that can be obtained using the present invention is to simplify the process and reduce costs.

The technical result is achieved by using a method of obtaining calcium stearate interaction of stearic acid, previously dissolved in water-ethanol solution, and calcium hydroxide with heating and vigorous stirring, followed by filtration and drying the precipitate, and the interaction of stearic acid and calcium hydroxide is carried out in aqueous medium, and the emulsion is heated to 58-65°C, transferred to a stable emulsion is maintained at this temperature for 20-40 minutes to pH 8.0-9.0 solution, carry out the heat treatment for mounting particles, then with constant stirring, the temperature was raised to 70-85°C, incubated for 10-15 minutes to pH 7.5-9.0 solution, pour water, mix and filter.

The method of obtaining calcium stearate is as follows.

In the reactor (not shown) loaded acrylic balls, then pumped potable water, loaded stearic acid and calcium hydroxide, with constant stirring, the emulsion is heated to 58-65°C, translating into a stable emulsion direct synthesis, and maintained at this temperature during the s 20-40 minutes, control the temperature, at the end of the excerpts selected a sample of a suspension of calcium stearate to determine the pH of the mother liquor, which is equal to 8.0, and 9.0, in the case of a failure analysis is performed adjustment of the synthesis calculation additives calcium hydroxide and stearic acid, while to complete the synthesis of calcium stearate carry out the heat treatment of the suspension with the aim of building block design (enlarged) product particles, which improves filtering the suspension with constant stirring of the suspension in the reactor temperature was raised to 70-85°C and maintained at this temperature for at least 10-15 minutes after the heat treatment, the pH of the mother liquor is in the range of 7.5-9.0 and in the reactor pour potable water, mix and prepared suspension of calcium stearate send on stage filtering

in the process of filtering the paste of calcium stearate are cut and served on the stage drying calcium stearate, the temperature of the drying agent is 100-150°C and its control, support 70-90°C, the dried product in the form of a dusty mixture enters the cyclone (not shown) of the type SCL-42, where the air-dust mixtures are separated the main part of the product, while newbeny product is mixed with air enters the bag filter (not shown), where the delayed filter t is the sand bags then the finished product is calcium stearate analyze for compliance with THE 2432-005-102-69-039-05 the following brands:

- PVC stabilizers, grades C-17, C, D;

- brand BUT;

- "clean".

The stearates of calcium grades of C-17, BUT "clean" is a white powder with a slightly yellowish tinge, insoluble in water, soluble in mineral acids and concentrated alkalis and calcium stearate brand D - white powder with a yellowish tinge, prone to cachemate.

The stearates of calcium stabilizers PVC grades of C-17, C, D, BUT is used as a thermo stabilizer in the production of polyvinyl chloride resins in the processing of plastics, in the manufacture of artificial leather and linoleum.

Calcium stearate brand "pure" is used in the production of vitamin tablets and medicines, as well as for scientific purposes, then the finished product is Packed and Packed.

A brief description of the drawings and other materials

The following table presents a method of obtaining calcium stearate, physico-chemical characteristics of calcium stearate.

The implementation of the invention

Example. In the reactor (not shown) download 70-120 kg acrylic balls, then pumped 2.0 to 2.5 m of potable water, load 450 kg of stearic acid and 66,2 kg of calcium hydroxide, with the weight determined by the label on the container or when the mandatory weigh-in, n is the sample, on the scales VM-150, with constant stirring, the emulsion is heated to 58-65°C, translating into a stable emulsion direct synthesis, and maintained at this temperature for 20-40 minutes, the temperature control is carried out with the help of the device, for example, "Drive-250", at the end of the excerpts selected a sample of a suspension of calcium stearate to determine the pH of the mother liquor, which is equal to 8.0, and 9.0, in the case of a failure analysis is performed adjustment of the synthesis calculation additives calcium hydroxide and stearic acid, while to complete the synthesis of calcium stearate carry out the heat treatment of the suspension with the aim of building block approach (escalation) particles of the product, which helps to improve filtering the suspension with constant stirring of the suspension in the reactor temperature was raised to 70-85°C and maintained at this temperature for at least 10-15 minutes after the heat treatment, the pH of the mother liquor is in the range of 7.5-9.0 and in the reactor pour 0.5 m3potable water, mix and prepared suspension of calcium stearate send on stage filtration, process filtration pasta calcium stearate cut and served on the stage drying calcium stearate, and received in the process of filtering the washing water is served in the collection located and then used in the preparation of SYN is Esav, the dilution of the suspension, slyvka technological equipment and so on. Drying the paste of calcium stearate is carried out in the drying units (not shown) of the type "CS" ("Boiling layer"), wet pasta product is fed to the grid of the drying unit, then the drying agent (air) served under lattice drying units, the flow rate of the drying agent control unit - flow indicator, temperature of the drying agent is 100-150°C and its control, for example, the device "Drive-250", temperature, "KS" support 70-90°C, the dried product in the form of a dusty mixture enters the cyclone (not shown) of the type SCL-42 where dusty mixture separated the main part of the product, while newbeny product is mixed with air enters the bag filter (not shown), where the delayed filter cloth sleeve, then the finished product is calcium stearate analyze for compliance with THE 2432-005-102-69-039-05 the following brands:

- PVC stabilizers, grades C-17, C, D;

- brand BUT;

- "clean".

The stearates of calcium grades of C-17, BUT "clean" is a white powder with a slightly yellowish tinge, insoluble in water, soluble in mineral acids and concentrated alkalis and calcium stearate brand D - white powder with a yellowish tinge, prone to cachemate.

The chemical formula of the product is - CaSt2·H2Oh, where

St - the symbol of the balance of fatty acids with the General formula: CnH2n+1Soo.

In the case of the use of stearin - n=18.

When using a mixture of stearin and synthetic fatty acids (FFA) fraction17-C30indicator - n=17-20.

Molecular weight of calcium stearate:

- qualified clean - 625,04;

- qualification of PVC stabilizers, brand-17-633,3-592,3 depending on the acid number of FLC.

The stearates of calcium stabilizers PVC grades of C-17, C, D, BUT is used as a thermo stabilizer in the production of polyvinyl chloride resins in the processing of plastics, in the manufacture of artificial leather and linoleum.

Calcium stearate brand "pure" is used in the production of vitamin tablets and medicines, as well as for scientific purposes, while calcium stearate qualification "clean" is obtained on the basis of stearin technical I and II varieties or imported, PVC stabilizers, all grades - based on the solid stearin or a mixture of stearin technical and FFA fractions With17-C20the output of calcium stearate 99, 55%, according to the physical-chemical indicators of calcium stearate meet the requirements and standards specified in the table for stabilizers brand "pure". C-17, D, C, BUT then the finished product is served in the bins (not shown) of the finished product to follow what their packing and packaging.

The present invention in comparison with the prototype and other known technical solution has the following advantages:

- simplification of the technological process;

- cost reduction.

The method of obtaining calcium stearate interaction of stearic acid and calcium hydroxide with heating and vigorous stirring, followed by filtration and drying the precipitate, wherein the interaction of stearic acid and calcium hydroxide is carried out in aqueous medium, and the emulsion is heated to 58-65°C, transferred to a stable emulsion is maintained at this temperature for 20-40 minutes to pH 8.0-9.0 solution, carry out the heat treatment for mounting particles with constant stirring, the temperature was raised to 70-85°C, incubated for 10-15 minutes to pH 7.5-9.0 solution, pour water, mix and filter.



 

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8 cl, 5 ex, 2 dwg

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3 ex

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3 ex

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2 cl, 1 tbl, 1 ex

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6 cl, 1 dwg, 1 ex

FIELD: chemistry.

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15 cl, 16 ex

FIELD: chemistry.

SUBSTANCE: maleic acid derivatives having general formula

have metallo-β-lactamase inhibiting activities. It is possible to recover anti-bacterial activities of β-lactam antibiotics against metallo-β-lactamase producing bacteria by combining the compound of general formula (I) with β-lactam antibiotics. The metallo-β-lactamase inhibitor is a compound of formula (I) or a pharmaceutically acceptable salt thereof, wherein R1 denotes C2-6-alkyl; C3-7-cycloalkyl, where said cycle can be substituted with a hydroxyl group or can be condensed with an aryl; hydroxymethyl; - C1-3-alkylene phenyl, where said phenyl group can be substituted with a hydroxyl group, C1-6-alkyl group, hydroxymethyl group, a -COOM group, where M denotes a hydrogen atom or a pharmaceutically acceptable cation, a -CO-NR22R23 group, where R22 and R23, which can be identical or different, denote a hydrogen atom or C1-6-alkyl, wherein the alkyl can additionally be substituted with an aminocarbonyl, or R22 and R23, together with a nitrogen atom with which they are bonded, can form a five- or six-member saturated heterocyclic ring containing 1-2 oxygen or nitrogen atoms, and the heterocycle can be substituted with a hydroxyl group or a C1-6-alkanoyloxy group, a -O-R24 group, where R24 denotes C1-6-alkyl, wherein the alkyl is optionally substituted with an aminocarbonyl, an amine group, a guanidine group or a five- or six-member saturated heterocycle, having 1-2 nitrogen atoms, -COOM, where M denotes a hydrogen atom, C1-6-alkyl or a pharmaceutically acceptable cation, or a five- or six-member unsaturated heterocycle, having 1-2 nitrogen atoms; - C0-1 alkylene heterocycle, where said heterocycle is a five- or six-member saturated or unsaturated heterocycle containing one nitrogen or oxygen atom and can be substituted with a hydroxyl group; - O-C1-6-alkyl; or - S-C1-6-alkyl, R2 denotes C1-6-alkyl, C3-7-cycloalkyl, where said cycle can be substituted with a hydroxyl group or can be condensed with an aryl; or - C1-3-alkylene phenyl, each M1 independently denotes a hydrogen atom, a pharmaceutically acceptable cation.

EFFECT: new metallo-β-lactamase inhibitor acts as a medicament for inhibiting inactivation of β-lactam antibiotics and recovering anti-bacterial activities.

18 cl, 3 tbl, 98 ex

FIELD: chemistry.

SUBSTANCE: invention relates to chemistry of platinum metals, particularly synthesis of palladium compounds, specifically synthesis of heteronuclear acetates of palladium with non-ferrous metals. The method of producing heteronuclear acetates of palladium with non-ferrous metals involves reaction of an acetate compound of palladium and a non-ferrous metal compound in a glacial acetic acid solution, where the reaction of compounds, taken in molar ratio palladium: non-ferrous metal of 1:(0.90-0.97), takes place in glacial acetic acid used in amount of (600-800)% of the molar amount of palladium, at temperature (70-90)°C with evaporation of the solvent to wet or dry residue, with repeated addition of glacial acetic acid in amount of (200-600)% of the molar amount of palladium, repeated evaporation of the solvent at temperature (80-120)°C, with treatment of the dry residue, pre-heated to (70-90)°C, with a solution of a mixture of benzene or toluene and acetic acid anhydride with volume ratio thereof equal to (4-8):1 respectively, the amount of the acetic acid anhydride being equal to (20-60)% of the molar amount of palladium, at temperature (70-100)°C for (2-30) minutes, cooling the obtained suspension to temperature (40-70)°C and filtering the desired compound. In another version, the method involves reaction of a palladium acetate and an acetate compound of a non-ferrous metal in glacial acetic acid solution with solvent evaporation, where the reaction of compounds, taken in molar ratio palladium: non-ferrous metal equal to 1:(0.90-0.97), takes place in glacial acetic acid used in amount of (400-600)% of the molar amount of palladium, at temperature (80-120)°C with solvent evaporation to a dry residue, with subsequent treatment thereof with a solution of a mixture of benzene or toluene and acetic acid anhydride, pre-heated to (70-90)°C, with volume ratio thereof equal to (4-8):1 respectively, the acetic acid anhydride being in amount of (20-60)% of the molar amount of palladium, at temperature (70-100)°C for (2-30) minutes, cooling the obtained suspension to temperature (40-70)°C and filtering the desired compound.

EFFECT: invention enables to realise a simple and stable method of producing desired compounds with high output.

4 cl, 46 ex, 2 tbl

FIELD: organic chemistry, chemical technology, agriculture.

SUBSTANCE: invention relates to a method for preparing the preparation comprising triterpenic acid water-soluble salts and additionally added protein-containing product and vegetable raw, the source of triterpenic acids taken in the following ratio of components, wt.-%: protein-containing product, 10-17; triterpenic acid sodium salts, 4-5, and vegetable raw, the balance. Method involves mixing triterpenic acid-containing vegetable raw with the protein-containing product taken in the ratio = (9-11):(1-2), mechanical-chemical treatment of this mixture in activator device, mixing of prepared semi-finished product with sodium carbonate or sodium hydrocarbonate taken in the ratio = (92-97):(3.5-8.3) and repeated treatment in the activator device. Method involves applying flow-type ball vibration-centrifugal or ellipse-centrifugal mills as the activator device that provide the acceleration of milling bodies up to 170-250 m/c2 and time for treatment for 1.5-3 min. Invention provides simplifying the process and the complex processing waste in lumber industry.

EFFECT: improved preparing method.

6 cl, 1 tbl, 6 ex

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