CN104529747A - Purification method of dodecanedioic acid - Google Patents
Purification method of dodecanedioic acid Download PDFInfo
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- CN104529747A CN104529747A CN201410830623.1A CN201410830623A CN104529747A CN 104529747 A CN104529747 A CN 104529747A CN 201410830623 A CN201410830623 A CN 201410830623A CN 104529747 A CN104529747 A CN 104529747A
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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Abstract
The invention relates to a purification method of dodecanedioic acid, belonging to purification treatment of cycle-free dicarboxylic acid with 12 carbon atoms. The method is characterized by comprising the following steps: by using a dodecanedioic acid crude product produced by microbial fermentation as an initial raw material and water as a dissolving solvent, carrying out alkali fusion at 100-102 DEG C under the condition of pH value of 6.0-6.2 to prepare a dodecanedioic acid crude product water solution; and after carrying out adsorption-oxidation dual decolorization, acidifying at 98-102 DEG C to crystallize, and finally, drying to obtain the scale-like high-purity dodecanedioic acid crystal product. The purification method of dodecanedioic acid has the advantages of favorable product color, high product purity, high refinement yield, equipment investment saving and resource saving, and is simple to operate and beneficial to environmental protection. The purification yield of the dodecanedioic acid is greater than or equal to 98.4%. The dodecanedioic acid is suitable to be used as a polycondensation monomer to perform polycondensation reaction with diamine to synthesize the long-carbon-chain nylon, and is also suitable to be used as a raw material of synthetic perfume and drugs.
Description
Technical field
The present invention is a kind of purification process of dodecanedioic acid.Belong to the purification process of the acyclic di-carboxylic acid having 12 carbon atoms.
Background technology
Dodecanedioic acid (Dodecanedioic Acid) has another name called bay diacid.In long-chain biatomic acid, develop Industrial products comparatively early.Be mainly used in synthesized polymer material, spices, medicine etc.Wherein, synthesizing long carbon chain nylon (also known as polyamide resin) engineering plastics as polycondensation monomer and diamine generation polycondensation, is one of most important purposes.
Nylon is the family macromolecule compound containing acid amides group (-NHCO-) on molecular backbone chain.Due in nylon molecules structure containing a large amount of amide group, macromole end be amino or carboxyl, thus be the strong polarity of a class, intermolecular energy formation hydrogen bond and there is the crystalline polymer of certain reactive behavior.Nylon is the one that in five large-engineering plastics (nylon, polyoxymethylene, polycarbonate, polyphenylene oxide, polybutylene terephthalate), consumption is maximum, kind maximum, purposes is the widest, qualification is the oldest,
The distinctive molecular machinery of long-chain nylon, give the over-all properties that it is good, intensity is higher than metal, excellent mechanical property, thermotolerance, wearability, chemical resistant properties, flame retardant resistance and self lubricity, frictional coefficient is low and easily process, and it can be processed into various plastics, also wire drawing can make fiber, can also make film, coating and tackiness agent etc.Be widely used in automobile, electric, mechanical, communication, the field such as military affairs and aerospace.
Take dodecanedioic acid as raw material, as the long carbon chain nylon that polycondensation monomer and diamine generation polycondensation synthesize, mainly contain nylon 12, nylon 612, nylon 11 12 and nylon 1212 etc.,
In recent years, the demand of dodecanedioic acid on international and domestic market increases sharply, and rises year by year.And, the requirement of the various technical performance index of quality product is improved constantly, more and more harsher.Commercially available dodecanedioic acid can not meet the requirement of long-chain nylon technique to the technical indicator of its purity and visual appearance each side.
In prior art, the purification process of dodecanedioic acid mainly with the dodecanedioic acid crude product of Production by Microorganism Fermentation for starting raw material, adopt solvent method to carry out purification by recrystallization.The solvent adopted mainly contains Glacial acetic acid and methyl alcohol, exists following not enough:
1. methyl alcohol, Glacial acetic acid price are higher, solvent recuperation, and circulating-use equipment investment is large.
2. there are the following problems as recrystallisation solvent for methyl alcohol,
1.. because methyl alcohol easy and solute dodecanedioic acid generation esterification under acidity and heating condition, add new impurity, add the load of purifying.Reduce the yield of dodecanedioic acid.
2.. because the solubleness of dodecanedioic acid in methyl alcohol is comparatively large, in recrystallization process, always have a small amount of dodecanedioic acid product to dissolve in a solvent, cause the yield of product low, production cost is high.
3. adopt acetic acid as solvent, there is acetic acid residual comparatively large in filtered liquid, the problem that product yield is not high.
4. acetic acid, methyl alcohol are all volatile, cause environmental pollution.
A kind of product color is good, purifying is high, and refining yield is high, low equipment investment, easy and simple to handle, and economize on resources, the purification process being conducive to the dodecanedioic acid of environment protection is that people expected.
Summary of the invention
The object of the invention is to avoid above-mentioned weak point of the prior art, and provide that a kind of product color is good, purifying is high, refining yield is high, low equipment investment, easy and simple to handle, economizes on resources, is conducive to the purification process of the dodecanedioic acid of environment protection.。
Object of the present invention can be reached by following measure:
The purification process of dodecanedioic acid of the present invention, it is characterized in that with the dodecanedioic acid crude product of Production by Microorganism Fermentation for starting raw material, using water as dissolution solvent, temperature 100 ~ 102 DEG C, under pH value 6.0 ~ 6.2 condition, alkali is molten, prepares the dodecanedioic acid crude product aqueous solution; Again by after absorption, being oxidized dual decolouring, acid out crystallization at 98 ~ 102 DEG C of temperature, finally, dries obtained fish scale-shaped High-pure Dodecanedioic Acid crystal product.
Adopt under 100 ~ 102 DEG C of higher temperatures with water as solvent, under pH value 6.0 ~ 6.2 condition, alkali is molten, prepare the dodecanedioic acid crude product aqueous solution, improve the solubleness of diprotic acid and sodium salt thereof, greatly reduce the consumption of the liquid caustic soda dissolving diprotic acid, when last acid out, the consumption of corresponding dilute sulphuric acid also can greatly reduce, thus decrease the generation of salinity in system, product more easily washs, making final crystal decrease the consumption of deionized water when washing, reducing the ash content of product, improve the purity of product.
Adsorb, be oxidized dual decolouring, enhance decolorizing effect, greatly reduce the colourity of product.
At 98 ~ 102 DEG C of temperature, acid out crystallization, acid out temperature is higher, reduces the speed that crystal is separated out, is conducive to the growth of nucleus, decreases for the coated of impurity and carrying secretly in product crystal, thus increases grain-size, improve the purity of product.Quality product can meet the requirement of long-chain nylon technique to the technical indicator of its purity and visual appearance each side.
The present invention adopts deionization water as solvent, deionized water is cheap and easy to get, nonpoisonous and tasteless, environmental protection, to avoid in prior art Glacial acetic acid and alcohol organic solvent to the pollution of environment, and the solubleness of dodecanedioic acid in water is very little, product residual in last mother liquor is few, create the effect that product yield is significantly improved, synchronously reduce production cost.Significantly improve the economic benefit of enterprise, facilitate the development of dodecanedioic acid industry effectively.Thus complete task of the present invention.
Object of the present invention can also be reached by following measure:
The purification process of dodecanedioic acid of the present invention, is characterized in that the processing condition of concrete purification refine processing step and each step are as follows:
1. .. adsorption bleaching
In solubilizing reaction still, drop into deionized water 1000 weight part, crude product dodecanedioic acid is added in dry measure 180 weight part under stirring, add aqueous sodium hydroxide solution 110 ~ 120 weight part that mass concentration is 30 ~ 31%, be warming up to 100 ~ 102 DEG C, pH value controls between 6.0 ~ 6.2, after material dissolves completely, add coconut husk type gac 3 ~ 5 weight part, insulation decolouring 20 ~ 30 minutes;
2. .. oxidative decoloration
By the material filtered while hot after 1. processing through step, filter cake is with 85 ~ 90 DEG C of hot water injections, and filtrate and washing fluid put into oxidative decoloration reactor in the lump, are warming up to 98 ~ 100 DEG C, and at this temperature, control in 5 ~ 10 minutes, add the hydrogen peroxide that mass content is 30%, under stirring, carry out oxidative decoloration, at 98 ~ 100 DEG C of temperature, insulation oxidation 2 ~ 3 hours, standby acidizing crystal;
3.. high temperature acidified crystallization
A. the configuration of dilute sulphuric acid
In dilute sulphuric acid preparation still, add deionized water 105 ~ 120 weight part, under cooling, stirring, slowly drip the vitriol oil of 98.5%, be mixed with the dilute sulphuric acid that mass percentage concentration is 25 ~ 30%, be cooled to room temperature, standby crystallization;
B. acid out crystallization
The dilute sulphuric acid of step a is configured 25 ~ 30%, slowly add under stirring step 2. process after the dodecanedioic acid aqueous solution in, time 1.5 hours, control acid out temperature between 98 ~ 102 DEG C, crystallization time 1.5 ~ 2 hours, along with adding of dilute sulphuric acid, fish scale-shaped crystallization is constantly had in solution, control pH value=3.0 at the end of acidifying, acid adding is complete, insulated and stirred 15 ~ 20 minutes, decrease temperature crystalline, cooling is stopped when temperature is down to 25 DEG C, vacuum filtration, with 500 ~ 520 parts by weight of deionized water washing leaching cakes, washings reclaims, solvent cycle as next batch uses,
4. dry
Filter cake after the step 3. vacuum filtration of b item, dries at 100 ~ 105 DEG C of temperature;
Obtained fish scale-shaped High-pure Dodecanedioic Acid crystal; Product yield >=98.4%; Quality product reaches following technical indicator:
It is the preferred technical scheme of the purification process of dodecanedioic acid of the present invention.
The purification process of dodecanedioic acid of the present invention, is characterized in that the processing condition of concrete purification refine processing step and each step are as follows:
1. .. adsorption bleaching
In solubilizing reaction still, drop into deionized water 1000 weight part, crude product dodecanedioic acid is added in dry measure 180 weight part under stirring, add aqueous sodium hydroxide solution 110 weight part that mass concentration is 30.3%, be warming up to 100 ~ 102 DEG C, pH value controls between 6.0 ~ 6.2, after material dissolves completely, add coconut husk type gac 3 weight part, insulation decolouring 30 minutes;
2. .. oxidative decoloration
By the material filtered while hot after 1. processing through step, filter cake is with 90 DEG C of hot water injections, and filtrate and washing fluid put into oxidative decoloration reactor in the lump, are warming up to 98 ~ 100 DEG C, and at this temperature, control in 5 ~ 10 minutes, add the hydrogen peroxide that mass content is 30%, under stirring, carry out oxidative decoloration, at 98 ~ 100 DEG C of temperature, insulation oxidation 2 hours, standby acidizing crystal;
3.. acid out crystallization
A. the configuration of dilute sulphuric acid
In dilute sulphuric acid preparation still, add deionized water 105 weight part, under cooling, stirring, slowly drip the vitriol oil of 98.5%, be mixed with the dilute sulphuric acid that mass percentage concentration is 25 ~ 30%, be cooled to room temperature, standby crystallization;
B. acidifying, crystallization
The dilute sulphuric acid of step a is configured 25 ~ 30%, slowly add under stirring step 2. process after the dodecanedioic acid aqueous solution in, time 1.5 hours, control acid out temperature between 98 ~ 102 DEG C, crystallization time 1.5 hours, along with adding of dilute sulphuric acid, fish scale-shaped crystallization is constantly had in solution, control pH value=3.0 at the end of acidifying, acid adding is complete, insulated and stirred 15 ~ 20 minutes, decrease temperature crystalline, cooling is stopped when temperature is down to 25 DEG C, vacuum filtration, with 500 parts by weight of deionized water washing leaching cakes, washings reclaims, solvent cycle as next batch uses,
4. dry
Filter cake after the step 3. vacuum filtration of b item, dries at 100 ~ 105 DEG C of temperature;
Obtained fish scale-shaped High-pure Dodecanedioic Acid crystal; Product yield >=98.6%; Quality product reaches following technical indicator:
It is a preferred technical scheme.
The application of dodecanedioic acid product prepared by the purification process of dodecanedioic acid of the present invention, is characterized in that being applicable to synthesize long carbon chain nylon as polycondensation monomer and diamine generation polycondensation; Also the raw material of synthetic perfume, medicine is applicable to.
The purification process of the dodecanedioic acid of invention, has following positively effect compared to existing technology:
1. provide that a kind of product color is good, purifying is high, refining yield is high, low equipment investment, easy and simple to handle, economizes on resources, is conducive to the purification process of the dodecanedioic acid of environment protection.Successfully solve problems of the prior art.
2. adopt under 100 ~ 102 DEG C of higher temperatures with water as solvent, under pH value 6.0 ~ 6.2 condition, alkali is molten, prepare the dodecanedioic acid crude product aqueous solution, improve the solubleness of diprotic acid and sodium salt thereof, greatly reduce the consumption of the liquid caustic soda dissolving diprotic acid, when last acid out, the consumption of corresponding dilute sulphuric acid also can greatly reduce, thus decrease the generation of salinity in system, product more easily washs, making final crystal decrease the consumption of deionized water when washing, reducing the ash content of product, improve the purity of product.
3. adopt absorption, be oxidized dual decolouring, enhance decolorizing effect, greatly reduce the colourity of product, improve quality product.
4., at 98 ~ 102 DEG C of temperature, acid out crystallization, acid out temperature is higher, reduces the speed that crystal is separated out, is conducive to the growth of nucleus, decreases for the coated of impurity and carrying secretly in product crystal, thus increases grain-size, improve the purity of product.
5. quality product can meet the requirement of long-chain nylon technique to the technical indicator of its purity and visual appearance each side.
6. the present invention adopts deionization water as solvent, deionized water is cheap and easy to get, nonpoisonous and tasteless, environmental protection, to avoid in prior art Glacial acetic acid and alcohol organic solvent to the pollution of environment, and the solubleness of dodecanedioic acid in water is very little, product residual in last mother liquor is few, create the effect that product yield is significantly improved, synchronously reduce production cost.Significantly improve the economic benefit of enterprise, facilitate the development of dodecanedioic acid industry effectively.
7. purification yield >=98.4% of dodecanedioic acid,
Embodiment
The present invention will now be further detailed embodiment:
Embodiment 1
A kind of process for purification improving dodecanedioic acid purity and yield of the present invention, comprises following operation steps:
1. .. adsorption bleaching
In solubilizing reaction still, drop into deionized water 1000 weight part, crude product dodecanedioic acid is added in dry measure 180 weight part under stirring, add aqueous sodium hydroxide solution 110 weight part that mass concentration is 30.3%, be warming up to 100 DEG C, pH value controls between 6.0, after material dissolves completely, add coconut husk type gac 3 weight part, insulation decolouring 20 minutes;
2. .. oxidative decoloration
By the material filtered while hot after 1. processing through step, filter cake is with 90 DEG C of hot water injections, and filtrate and washing fluid put into oxidative decoloration reactor in the lump, are warming up to 98 DEG C, and at this temperature, control in 5 ~ 10 minutes, add the hydrogen peroxide that mass content is 30%, under stirring, carry out oxidative decoloration, at 98 ~ 100 DEG C of temperature, insulation oxidation 2 hours, standby acidizing crystal;
3.. acid out crystallization
A. the configuration of dilute sulphuric acid
In dilute sulphuric acid preparation still, add deionized water 105 weight part, under cooling, stirring, slowly drip the vitriol oil 40 weight part of 98.5%, be mixed with the dilute sulphuric acid that mass percentage concentration is 27.2%, be cooled to room temperature, standby crystallization;
B. acidifying, crystallization
The dilute sulphuric acid of step a is configured 27.2%, slowly add under stirring step 2. process after the dodecanedioic acid aqueous solution in, control acid out temperature at 98 DEG C, crystallization time 1.5 hours, along with adding of dilute sulphuric acid, fish scale-shaped crystallization is constantly had in solution, control pH value=3.0 at the end of acidifying, acid adding is complete, insulated and stirred 15 minutes, decrease temperature crystalline, stop cooling when temperature is down to 25 DEG C, vacuum filtration, with 500 parts by weight of deionized water washing leaching cakes, washings reclaims, and the solvent cycle as next batch uses;
4. dry
Filter cake after the step 3. vacuum filtration of b item, dries at 100 ~ 105 DEG C of temperature;
Obtained fish scale-shaped High-pure Dodecanedioic Acid crystal 178 weight part; Product yield 98.9%; Quality product reaches following technical indicator:
Embodiment 2
A kind of process for purification improving dodecanedioic acid purity and yield of the present invention, comprises following operation steps:
1. .. adsorption bleaching
In solubilizing reaction still, drop into deionized water 1000 weight part, crude product dodecanedioic acid is added in dry measure 180 weight part under stirring, add aqueous sodium hydroxide solution 110 weight part that mass concentration is 30.3%, be warming up to 101 DEG C, pH value controls between 6.1, after material dissolves completely, add coconut husk type gac 4 weight part, insulation decolouring 30 minutes;
2. .. oxidative decoloration
By the material filtered while hot after 1. processing through step, filter cake is with 85 DEG C of hot water injections, and filtrate and washing fluid put into oxidative decoloration reactor in the lump, are warming up to 99 DEG C, and at this temperature, control in 5 ~ 10 minutes, add the hydrogen peroxide that mass content is 30%, under stirring, carry out oxidative decoloration, at 98 ~ 100 DEG C of temperature, insulation oxidation 3 hours, standby acidizing crystal;
3.. acid out crystallization
A. the configuration of dilute sulphuric acid
In dilute sulphuric acid preparation still, add deionized water 120 weight part, under cooling, stirring, slowly drip the vitriol oil 42 weight part of 98.5%, be mixed with the dilute sulphuric acid that mass percentage concentration is 28.1%, be cooled to room temperature, standby crystallization;
B. acidifying, crystallization
The dilute sulphuric acid of step a is configured 28.1%, slowly add under stirring step 2. process after the dodecanedioic acid aqueous solution in, control acid out temperature at 102 DEG C, crystallization time 2 hours, along with adding of dilute sulphuric acid, fish scale-shaped crystallization is constantly had in solution, control pH value=3.0 at the end of acidifying, acid adding is complete, insulated and stirred 15 minutes, decrease temperature crystalline, stop cooling when temperature is down to 25 DEG C, vacuum filtration, with 520 parts by weight of deionized water washing leaching cakes, washings reclaims, and the solvent cycle as next batch uses;
4. dry
Filter cake after the step 3. vacuum filtration of b item, dries at 100 ~ 105 DEG C of temperature;
Obtained fish scale-shaped High-pure Dodecanedioic Acid crystal 177.5 weight part; Product yield 98.6%; Quality product reaches following technical indicator:
Embodiment 3
A kind of process for purification improving dodecanedioic acid purity and yield of the present invention, comprises following operation steps:
1. .. adsorption bleaching
In solubilizing reaction still, drop into deionized water 1000 weight part, crude product dodecanedioic acid is added in dry measure 180 weight part under stirring, add aqueous sodium hydroxide solution 110 weight part that mass concentration is 30.3%, be warming up to 102 DEG C, pH value controls between 6.2, after material dissolves completely, add coconut husk type gac 5 weight part, insulation decolouring 25 minutes;
2. .. oxidative decoloration
By the material filtered while hot after 1. processing through step, filter cake is with 88 DEG C of hot water injections, and filtrate and washing fluid put into oxidative decoloration reactor in the lump, are warming up to 100 DEG C, and at this temperature, control in 5 ~ 10 minutes, add the hydrogen peroxide that mass content is 30%, under stirring, carry out oxidative decoloration, at 98 ~ 100 DEG C of temperature, insulation oxidation 2.5 hours, standby acidizing crystal;
3.. acid out crystallization
A. the configuration of dilute sulphuric acid
In dilute sulphuric acid preparation still, add deionized water 105 weight part, under cooling, stirring, slowly drip the vitriol oil 40 weight part of 98.5%, be mixed with the dilute sulphuric acid that mass percentage concentration is 27.2%, be cooled to room temperature, standby crystallization;
B. acidifying, crystallization
The dilute sulphuric acid of step a is configured 27.2%, slowly add under stirring step 2. process after the dodecanedioic acid aqueous solution in, control acid out temperature at 98 DEG C, crystallization time 2 hours, along with adding of dilute sulphuric acid, fish scale-shaped crystallization is constantly had in solution, control pH value=3.0 at the end of acidifying, acid adding is complete, insulated and stirred 15 minutes, decrease temperature crystalline, stop cooling when temperature is down to 25 DEG C, vacuum filtration, with 510 parts by weight of deionized water washing leaching cakes, washings reclaims, and the solvent cycle as next batch uses;
4. dry
Filter cake after the step 3. vacuum filtration of b item, dries at 100 ~ 105 DEG C of temperature;
Obtained fish scale-shaped High-pure Dodecanedioic Acid crystal 177.2 weight part; Product yield 98.4%; Quality product reaches following technical indicator:
Claims (4)
1. the purification process of a dodecanedioic acid, it is characterized in that with the dodecanedioic acid crude product of Production by Microorganism Fermentation for starting raw material, using water as dissolution solvent, temperature 100 ~ 102 DEG C, under pH value 6.0 ~ 6.2 condition, alkali is molten, prepares the dodecanedioic acid crude product aqueous solution; Again by after absorption, being oxidized dual decolouring, acid out crystallization at 98 ~ 102 DEG C of temperature, finally, dries obtained fish scale-shaped High-pure Dodecanedioic Acid crystal product.
2., according to the purification process of the dodecanedioic acid of claim 1, it is characterized in that the processing condition of concrete purification refine processing step and each step are as follows:
1. .. adsorption bleaching
In solubilizing reaction still, drop into deionized water 1000 weight part, crude product dodecanedioic acid is added in dry measure 180 weight part under stirring, add aqueous sodium hydroxide solution 110 ~ 120 weight part that mass concentration is 30 ~ 31%, be warming up to 100 ~ 102 DEG C, pH value controls between 6.0 ~ 6.2, after material dissolves completely, add coconut husk type gac 3 ~ 5 weight part, insulation decolouring 20 ~ 30 minutes;
2. .. oxidative decoloration
By the material filtered while hot after 1. processing through step, filter cake is with 85 ~ 90 DEG C of hot water injections, and filtrate and washing fluid put into oxidative decoloration reactor in the lump, are warming up to 98 ~ 100 DEG C, and at this temperature, control in 5 ~ 10 minutes, add the hydrogen peroxide that mass content is 30%, under stirring, carry out oxidative decoloration, at 98 ~ 100 DEG C of temperature, insulation oxidation 2 ~ 3 hours, standby acidizing crystal;
3.. high temperature acidified crystallization
A. the configuration of dilute sulphuric acid
In dilute sulphuric acid preparation still, add deionized water 105 ~ 120 weight part, under cooling, stirring, slowly drip the vitriol oil of 98.5%, be mixed with the dilute sulphuric acid that mass percentage concentration is 25 ~ 30%, be cooled to room temperature, standby crystallization;
B. acid out crystallization
The dilute sulphuric acid of step a is configured 25 ~ 30%, slowly add under stirring step 2. process after the dodecanedioic acid aqueous solution in, time 1.5 hours, control acid out temperature between 98 ~ 102 DEG C, crystallization time 1.5 ~ 2 hours, along with adding of dilute sulphuric acid, fish scale-shaped crystallization is constantly had in solution, control pH value=3.0 at the end of acidifying, acid adding is complete, insulated and stirred 15 ~ 20 minutes, decrease temperature crystalline, cooling is stopped when temperature is down to 25 DEG C, vacuum filtration, with 500 ~ 520 parts by weight of deionized water washing leaching cakes, washings reclaims, solvent cycle as next batch uses,
4. dry
Filter cake after the step 3. vacuum filtration of b item, dries at 100 ~ 105 DEG C of temperature;
Obtained fish scale-shaped High-pure Dodecanedioic Acid crystal; Product yield >=98.4%; Quality product reaches following technical indicator:
3., according to the purification process of the dodecanedioic acid of claim 1, it is characterized in that the processing condition of concrete purification refine processing step and each step are as follows:
1. .. adsorption bleaching
In solubilizing reaction still, drop into deionized water 1000 weight part, crude product dodecanedioic acid is added in dry measure 180 weight part under stirring, add aqueous sodium hydroxide solution 110 weight part that mass concentration is 30.3%, be warming up to 100 ~ 102 DEG C, pH value controls between 6.0 ~ 6.2, after material dissolves completely, add coconut husk type gac 3 weight part, insulation decolouring 30 minutes;
2. .. oxidative decoloration
By the material filtered while hot after 1. processing through step, filter cake is with 90 DEG C of hot water injections, and filtrate and washing fluid put into oxidative decoloration reactor in the lump, are warming up to 98 ~ 100 DEG C, and at this temperature, control in 5 ~ 10 minutes, add the hydrogen peroxide that mass content is 30%, under stirring, carry out oxidative decoloration, at 98 ~ 100 DEG C of temperature, insulation oxidation 2 hours, standby acidizing crystal;
3.. acid out crystallization
A. the configuration of dilute sulphuric acid
In dilute sulphuric acid preparation still, add deionized water 105 weight part, under cooling, stirring, slowly drip the vitriol oil of 98.5%, be mixed with the dilute sulphuric acid that mass percentage concentration is 25 ~ 30%, be cooled to room temperature, standby crystallization;
B. acidifying, crystallization
The dilute sulphuric acid of step a is configured 25 ~ 30%, slowly add under stirring step 2. process after the dodecanedioic acid aqueous solution in, time 1.5 hours, control acid out temperature between 98 ~ 102 DEG C, crystallization time 1.5 hours, along with adding of dilute sulphuric acid, fish scale-shaped crystallization is constantly had in solution, control pH value=3.0 at the end of acidifying, acid adding is complete, insulated and stirred 15 ~ 20 minutes, decrease temperature crystalline, cooling is stopped when temperature is down to 25 DEG C, vacuum filtration, with 500 parts by weight of deionized water washing leaching cakes, washings reclaims, solvent cycle as next batch uses,
4. dry
Filter cake after the step 3. vacuum filtration of b item, dries at 100 ~ 105 DEG C of temperature;
Obtained fish scale-shaped High-pure Dodecanedioic Acid crystal; Product yield >=98.6%; Quality product reaches following technical indicator:
4. the application of the dodecanedioic acid product prepared according to the purification process of the dodecanedioic acid of claim 1, is characterized in that being applicable to synthesize long carbon chain nylon as polycondensation monomer and diamine generation polycondensation; Also the raw material of synthetic perfume, medicine is applicable to.
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| WO2017088218A1 (en) | 2015-11-27 | 2017-06-01 | 希锐科技（北京）有限公司 | Method of co-producing long chain amino acid and dibasic acid |
| US10065921B1 (en) | 2017-07-07 | 2018-09-04 | Vitaworks Ip, Llc | Process for producing long chain amino acids and dibasic acids |
| CN109456172A (en) * | 2017-09-06 | 2019-03-12 | 中国石化扬子石油化工有限公司 | A kind of method of water phase purification dodecanedicarboxylic acid |
| US10343978B2 (en) | 2017-07-07 | 2019-07-09 | Vitaworks Ip, Llc | Process for producing long chain amino acids and dibasic acids |
| CN111848388A (en) * | 2019-04-29 | 2020-10-30 | 中国科学院微生物研究所 | Crystals of dodecanedioic acid and preparation method thereof |
| US10822300B2 (en) | 2017-07-07 | 2020-11-03 | Vitaworks Ip, Llc | Process for producing long chain amino acids and dibasic acids |
| WO2020251613A1 (en) | 2019-06-10 | 2020-12-17 | Vitaworks Ip, Llc | Producing long chain amino and dibasic acids |
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| US10343978B2 (en) | 2017-07-07 | 2019-07-09 | Vitaworks Ip, Llc | Process for producing long chain amino acids and dibasic acids |
| US10822300B2 (en) | 2017-07-07 | 2020-11-03 | Vitaworks Ip, Llc | Process for producing long chain amino acids and dibasic acids |
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| CN109456172B (en) * | 2017-09-06 | 2021-04-06 | 中国石化扬子石油化工有限公司 | Method for purifying dodecanedioic acid in water phase |
| CN111848388A (en) * | 2019-04-29 | 2020-10-30 | 中国科学院微生物研究所 | Crystals of dodecanedioic acid and preparation method thereof |
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