CN105541652A - Preparation method of cocoyl glutamate acid - Google Patents
Preparation method of cocoyl glutamate acid Download PDFInfo
- Publication number
- CN105541652A CN105541652A CN201510945430.5A CN201510945430A CN105541652A CN 105541652 A CN105541652 A CN 105541652A CN 201510945430 A CN201510945430 A CN 201510945430A CN 105541652 A CN105541652 A CN 105541652A
- Authority
- CN
- China
- Prior art keywords
- cocoyl
- temperature
- alcohol
- preparation
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/60—Preparation of carboxylic acid halides by conversion of carboxylic acids or their anhydrides or esters, lactones, salts into halides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of cocoyl glutamate acid. The preparation method comprises that phosgene as a raw material is fed into cocinic acid as a raw material in a micro-melting state at a temperature of 70-120 DEG C, the mixture undergoes a reaction in the presence of an organic amine catalyst for 5-30h, wherein a mole ratio of cocinic acid, phosgene to the catalyst of 1: 1.05-3.5: 0.05-0.2, the reaction product is subjected to reduced pressure vacuum distillation to form cocoyl chloride, at the room temperature, sodium glutamate is dissolved in a mixed solution of alcohol and water, wherein a mass ratio of the alcohol to water is 1: 1.0-10.0, cocoyl chloride and sodium hydroxide aqueous solutions are dropwisely added into the system in 0.5-6h under control of the system temperature in a range of 0-50 DEG C along with stirring, wherein a mole ratio of sodium amino acid salt to cocoyl chloride is 1: 1.0-1.6 and the system pH is kept in a range of 6-15 through a sodium hydroxide dropwise addition rate and use amount, the system is stirred for 0.5-6h, the solvent is subjected to reduced pressure removal at a temperature of 0-100 DEG C for 0.5-6h, the system is cooled, hydrochloric acid is slowly and dropwisely added into the system at a temperature of 0-50 DEG C along with stirring until crystals are precipitated, wherein the pH of the system is kept in a range of 0-10 through a hydrochloric acid dropwise addition amount, and the crystals are subjected to suction filtration and dried so that obtain the cocoyl glutamate acid is obtained. The preparation method has a simple preparation route, can be operated simply, is safe, has a high yield and can be easily industrialized.
Description
Technical field
The present invention relates to a kind of preparation method of cocoyl L-glutamic acid.
Background technology
In recent years, amino acid series tensio-active agent, with its security, biological degradability and excellent surfactivity, enjoys the concern of people.Cocoyl L-glutamic acid is made by the high material of security, very soft to skin, can not cause allergy and phototoxicity; Foam is suitable, and washing force is strong, has outstanding adaptability to hard water; Can fast decompose by biology; Cause containing lipid acid, therefore can make solution, micellelike obtains required viscosity.Because of its above-mentioned characteristic, be widely used in transparent system or (pearly-lustre) cleansing milk, shampoo, bath oil, soap, washing composition, shaving cream, toothpaste and industrial products, also can be used for the industry such as silk dyeing and finishing, rust-inhibiting additive, intermetallic composite coating, mineral floating and oil production.Preparing burden with other and have extensive compatibleness, is that other existing tensio-active agent lacks.It comes into operation over nearly 10 years by the U.S., Japan and Germany in a large number, and with the price exceeding raw materials cost many times marketing China.
Synthesis about cocoyl acyl glutamic acid does not almost have; meticulous with specialty chemicals technical progress 2003(23) report the synthetic method of N-lauroyl glutamate; the acetone that its solvent selects toxicity larger; due to the characteristic of amino acid series surfactivity product; residual acetone can cause product easily to turn to be yellow; the method long reaction time simultaneously; more than 18 hours; and aftertreatment purifying needs twice recrystallization; technology is loaded down with trivial details tediously long; not easy to operate, take time and effort, seriously run counter to environmental protection, safety object.
Summary of the invention
Its object of the present invention is just the preparation method providing a kind of cocoyl L-glutamic acid, has syntheti c route and respectively walks easy and simple to handle, that safety, reaction yield are high feature, and be easy to suitability for industrialized production.
Realize above-mentioned purpose and the technical scheme taked, comprise step,
1) with coconut oil photoreactive gas for raw material, be 1:1.05 ~ 3.5:0.05 ~ 0.2 by the mol ratio of coconut oil, phosgene and catalyzer, under organic amine catalyst effect, coconut oil leads to phosgene reaction 5 ~ 30 hours under 70 ~ 120 DEG C of micro-molten states, react complete, reduced vacuum distillation obtains described cocounut oil acyl chlorides;
2)under room temperature, be dissolved in by Sodium Glutamate in the mixing solutions of alcohol and water, the mass ratio of alcohol and water is 1:1.0 ~ 10.0, after dissolving, hierarchy of control temperature is 0 ~ 50 DEG C, under insulated and stirred, drip the aqueous solution of cocounut oil acyl chlorides and sodium hydroxide, the mol ratio of amino acid sodium and cocounut oil acyl chlorides is 1:1.0 ~ 1.6 simultaneously, time for adding about 0.5 ~ 6 hour, sodium hydroxide rate of addition and consumption maintain between 6 ~ 15 with system pH, drip and finish, and stir 0.5 ~ 6h; At maintaining the temperature at 0 ~ 100 DEG C, decompression desolventizing 0.5 ~ 6h; Cooling, temperature control, at 0 ~ 50 DEG C, under agitation, slowly drips hydrochloric acid, and the amount that hydrochloric acid drips maintains between 0 ~ 10 with system pH, and drip and finish, the crystallization of precipitate particle shape, suction filtration, after oven dry, obtains cocoyl L-glutamic acid.
Beneficial effect
Compared with prior art the present invention has the following advantages;
(1) cocounut oil acyl chlorides is produced by phosgenation, a large amount of phosphorus-containing wastewater can not be produced as chlorinating agent because of phosphorus trichloride, the sulfurous gas environmental pollution that sulfur oxychloride method produces is serious, hydrogenchloride that phosgenation produces can be made into hydrochloric acid and sells, carbonic acid gas can be used for preparing sodium carbonate, reach recycling, cost-saving effect;
(2) the present invention comes alternative acetone and water mixed solution and traditional pure aquatic system by adopting alcohol and water mixing solutions, avoid the generation of side reaction, solve the problem of product jaundice, improve product yield simultaneously, products obtained therefrom milder, smell, color and luster, better quality;
(3) the present invention is after the condensation stage terminates, and adopts the method for low temperature desolventizing agent and low temperature crystallization to replace the method for conventional high-temperature acidifying separatory, reduces the energy consumption in production, also greatly improves the security of operation while cost-saving;
(4) method of cocoyl L-glutamic acid prepared of the present invention, easy to operate, reaction yield is high, and easy suitability for industrialized production, substantially without the three wastes.
Embodiment
A preparation method for cocoyl L-glutamic acid, comprises step,
1) with coconut oil photoreactive gas for raw material, be 1:1.05 ~ 3.5:0.05 ~ 0.2 by the mol ratio of coconut oil, phosgene and catalyzer, under organic amine catalyst effect, coconut oil leads to phosgene reaction 5 ~ 30 hours under 70 ~ 120 DEG C of micro-molten states, react complete, reduced vacuum distillation obtains described cocounut oil acyl chlorides;
2)under room temperature, be dissolved in by Sodium Glutamate in the mixing solutions of alcohol and water, the mass ratio of alcohol and water is 1:1.0 ~ 10.0, after dissolving, hierarchy of control temperature is 0 ~ 50 DEG C, under insulated and stirred, drip the aqueous solution of cocounut oil acyl chlorides and sodium hydroxide, the mol ratio of amino acid sodium and cocounut oil acyl chlorides is 1:1.0 ~ 1.6 simultaneously, time for adding about 0.5 ~ 6 hour, sodium hydroxide rate of addition and consumption maintain between 6 ~ 15 with system pH, drip and finish, and stir 0.5 ~ 6h; At maintaining the temperature at 0 ~ 100 DEG C, decompression desolventizing 0.5 ~ 6h; Cooling, temperature control, at 0 ~ 50 DEG C, under agitation, slowly drips hydrochloric acid, and the amount that hydrochloric acid drips maintains between 0 ~ 10 with system pH, and drip and finish, the crystallization of precipitate particle shape, suction filtration, after oven dry, obtains cocoyl L-glutamic acid.
Described organic amide catalyzer is DMF, N,N-dimethylacetamide, pyridine or N, N-amide dimethyl butyrate, and preferred catalyzer is DMF.
Select alcohol solution to be solvent, described alcohol is the alcohols such as methyl alcohol, ethanol, propyl alcohol, Virahol, the trimethyl carbinol, isopropylcarbinol, and preferred alcohols is ethanol and Virahol.
Embodiment
The present invention, the first step produces cocounut oil acyl chlorides by phosgenation, its by product HCl and carbonic acid gas recyclable, use it for anything else, do not cause environmental pollution; Second step reaction solvent selects alcohol solution to replace aqueous acetone solution or pure aquatic system, and reactive behavior is good, and the reaction times is short, products obtained therefrom milder, better quality, not containing residual phosphorus, sulphur in product, can be widely used in the production of high-end tensio-active agent.
In the present invention, the implication of each term is explained as follows:
DEG C, temperature unit, degree Celsius; Mpa, pressure unit, 10
6pascal;
The present invention is realized by following proposal:
Step one, with coconut oil photoreactive gas for raw material, under organic amine catalyst effect, coconut oil leads to phosgene reaction 5 ~ 30 hours under 70 ~ 120 DEG C of micro-molten states, reacts complete, and reduced vacuum distillation obtains described cocounut oil acyl chlorides;
Step 2, under room temperature, be dissolved in by Sodium Glutamate in the mixing solutions of alcohol and water, after dissolving, hierarchy of control temperature is 0 ~ 50 DEG C, under insulated and stirred, drip the aqueous solution of cocounut oil acyl chlorides and sodium hydroxide, time for adding about 0.5 ~ 6 hour, sodium hydroxide rate of addition and consumption maintain between 6 ~ 15 with system pH simultaneously, drip and finish, stir 0.5 ~ 6h; At maintaining the temperature at 0 ~ 100 DEG C, decompression desolventizing 0.5 ~ 6h; Cooling, temperature control, at 0 ~ 50 DEG C, under agitation, slowly drips hydrochloric acid, and the amount that hydrochloric acid drips maintains between 0 ~ 10 with system pH, and drip and finish, the crystallization of precipitate particle shape, suction filtration, after oven dry, obtains cocoyl L-glutamic acid.
The synthetic method of described a kind of cocoyl L-glutamic acid, the organic amide catalyzer that step one is selected is DMF, N,N-dimethylacetamide, pyridine or N, N-amide dimethyl butyrate, and preferred catalyzer is DMF.
Step 2 selects alcohol and water mixing solutions to be solvent, and described alcohol is the alcohols such as methyl alcohol, ethanol, propyl alcohol, Virahol, the trimethyl carbinol, isopropylcarbinol, and preferred alcohols is ethanol and Virahol.
In above-mentioned synthetic method, step one, the mol ratio of coconut oil, phosgene and catalyzer is 1:1.05 ~ 3.5:0.05 ~ 0.2, the mol ratio of preferred coconut oil, phosgene and catalyzer is 1:1.05 ~ 1.5:0.05 ~ 0.1, and temperature of reaction is 70 ~ 120 DEG C, is preferably 70 ~ 80 DEG C, reaction times is 1 ~ 20 hour, be preferably 5 ~ 8 hours, react complete vacuum distilling and obtain cocounut oil acyl chlorides, distillation condition 140 ~ 180 DEG C (560Pa).
, preferred 1:3.0 ~ 6.0, amino acid sodium: the mol ratio of cocounut oil acyl chlorides is 1:1.0 ~ 1.6, and preferred mol ratio is 1:1.0 ~ 1.3, it is between 0 ~ 50 DEG C that system temperature controls, and is preferably 20 ~ 25 DEG C; Under agitation add cocounut oil acyl chlorides, add the aqueous sodium hydroxide solution of 40% simultaneously, reaction solution is between pH=6 ~ 15 always, and preferable ph controls 10 ~ 14, until add; Continue reaction 0.5 ~ 6h again, preferably 1 ~ 3 hour; In decompression removing process, control temperature is 0 ~ 100 DEG C, and be preferably 25 ~ 30 DEG C, the time is 0.5 ~ 6 hour, preferably 0.5 ~ 3 hour; Between cooling 0 ~ 50 DEG C, preferably 15 ~ 20 DEG C, drip hydrochloric acid under stirring, reaction solution is between pH=0 ~ 7 always, preferably 2 ~ 6, crystallization, suction filtration, after oven dry, obtains cocoyl L-glutamic acid.
Embodiment 1
Step one: to the 500ml there-necked flask that stirrer, thermometer, airway, reflux condensing tube are housed
In, add coconut oil 284g (1mol) successively, DMF 4.5g (0.06mol), be warming up to 80 DEG C, controlling temperature of reaction is 80 ~ 85 DEG C, passes into phosgene 105g (1.05mol), reacts complete in 5 ~ 8 hours, reduced vacuum is distilled, collect 140 ~ 180 DEG C of (560Pa) cuts, obtain cocounut oil acyl chlorides 265g, yield 90%.
Step 2: in the 1000ml there-necked flask that dropping funnel, thermometer, stirring are housed, add L-glutamic acid
Sodium 191g (1mol), be dissolved in 446g ethanol and water mixed solution (m ethanol: m water=1:4), stirring at normal temperature makes it dissolve, cocounut oil acyl chlorides is put into the dropping funnel of 500ml, water at low temperature bath temperature control, at 20 ~ 25 DEG C, under agitation adds cocounut oil acyl chlorides 359g (1.2mol), drip the aqueous sodium hydroxide solution of 40% simultaneously, make reacting liquid pH value maintain pH=10 ~ 12, drip and finish, continue to stir 2h; After end, rise to room temperature, decompression desolventizing 1h; Cooling, temperature control, at 15 ~ 20 DEG C, drips hydrochloric acid under stirring, makes system pH=6 ~ 8, the crystallization of precipitate particle shape, suction filtration, after oven dry, obtains cocoyl L-glutamic acid 339g, yield 92%.
Embodiment 2
Step one: the synthesis of cocounut oil acyl chlorides is with embodiment 1.
Step 2: in the 1000ml there-necked flask that dropping funnel, thermometer, stirring are housed, add L-glutamic acid
Sodium 191g (1mol), be dissolved in 446g ethanol and water mixed solution (m ethanol: m water=1:4), stirring at normal temperature makes it dissolve, cocounut oil acyl chlorides is put into the dropping funnel of 500ml, water at low temperature bath temperature control, at 15 ~ 20 DEG C, under agitation adds cocounut oil acyl chlorides 359g (1.2mol), drip the aqueous sodium hydroxide solution of 40% simultaneously, make reacting liquid pH value maintain pH=10 ~ 12, drip and finish, continue to stir 1h; After end, rise to room temperature, decompression desolventizing 1h; Cooling, temperature control, at 15 ~ 20 DEG C, drips hydrochloric acid under stirring, makes system pH=6 ~ 8, the crystallization of precipitate particle shape, suction filtration, after oven dry, obtains cocoyl L-glutamic acid 324g, yield 88%.
Embodiment 3
Step one: in the 500ml there-necked flask that stirrer, thermometer, airway, reflux condensing tube are housed,
Add coconut oil 284g (1mol) successively, N, dinethylformamide 4.5g (0.06mol), is warming up to 70 DEG C, and controlling temperature of reaction is 70 ~ 75 DEG C, pass into phosgene 110g (1.1mol), react complete in 5 ~ 8 hours, reduced vacuum is distilled, and collects 140 ~ 180 DEG C of (560Pa) cuts, obtain cocounut oil acyl chlorides 265g, yield 88%.
Step 2: in the 1000ml there-necked flask that dropping funnel, thermometer, stirring are housed, add L-glutamic acid
Sodium 191g (1mol), be dissolved in 356.8g ethanol and water mixed solution (m ethanol: m water=1:3), stirring at normal temperature makes it dissolve, cocounut oil acyl chlorides is put into the dropping funnel of 500ml, water at low temperature bath temperature control, at 10 ~ 13 DEG C, under agitation adds cocounut oil acyl chlorides 395g (1.3mol), drip the aqueous sodium hydroxide solution of 40% simultaneously, make reacting liquid pH value maintain pH=12 ~ 14, drip and finish, continue to stir 1h; After end, rise to room temperature, decompression desolventizing 3h; Cooling, temperature control, at 20 ~ 25 DEG C, drips hydrochloric acid under stirring, makes system pH=6 ~ 8, the crystallization of precipitate particle shape, suction filtration, after oven dry, obtains cocoyl L-glutamic acid 305g, yield 86%.
Embodiment 4
Step one: the synthesis of cocounut oil acyl chlorides is with embodiment 3.
Step 2: in the 1000ml there-necked flask that dropping funnel, thermometer, stirring are housed, add L-glutamic acid
Sodium 191g (1mol), be dissolved in 535.2g ethanol and water mixed solution (m ethanol: m water=1:5), stirring at normal temperature makes it dissolve, cocounut oil acyl chlorides is put into the dropping funnel of 500ml, water at low temperature bath temperature control, at 20 ~ 25 DEG C, under agitation adds cocounut oil acyl chlorides 359g (1.2mol), drip the aqueous sodium hydroxide solution of 40% simultaneously, make reacting liquid pH value maintain pH=12 ~ 14, drip and finish, continue to stir 2h; After end, rise to room temperature, decompression desolventizing 1.5h; Cooling, temperature control, at 20 ~ 25 DEG C, drips hydrochloric acid under stirring, makes system pH=4 ~ 6, the crystallization of precipitate particle shape, suction filtration, after oven dry, obtains cocoyl L-glutamic acid 331g, yield 90%.
Embodiment 5
Step one: in the 500ml there-necked flask that stirrer, thermometer, airway, reflux condensing tube are housed,
Add coconut oil 284g (1mol) successively, pyridine 4.8g (0.06mol), be warming up to 70 DEG C, controlling temperature of reaction is 70 ~ 75 DEG C, passes into phosgene 110g (1.1mol), reacts complete in 5 ~ 8 hours, reduced vacuum is distilled, collect 140 ~ 180 DEG C of (560Pa) cuts, obtain cocounut oil acyl chlorides 265g, yield 88%.
Step 2: in the 1000ml there-necked flask that dropping funnel, thermometer, stirring are housed, add L-glutamic acid
Sodium 191g (1mol), be dissolved in 446g ethanol and water mixed solution (m ethanol: m water=1:4), stirring at normal temperature makes it dissolve, cocounut oil acyl chlorides is put into the dropping funnel of 500ml, water at low temperature bath temperature control, at 20 ~ 25 DEG C, under agitation adds cocounut oil acyl chlorides 359g (1.2mol), drip the aqueous sodium hydroxide solution of 40% simultaneously, make reacting liquid pH value maintain pH=10 ~ 12, drip and finish, continue to stir 1h; After end, rise to room temperature, decompression desolventizing 1.5h; Cooling, temperature control, at 20 ~ 25 DEG C, drips hydrochloric acid under stirring, makes system pH=4 ~ 6, the crystallization of precipitate particle shape, suction filtration, after oven dry, obtains cocoyl L-glutamic acid 327g, yield 89%.
Embodiment 6
Step one: the synthesis of cocounut oil acyl chlorides is with embodiment 5.
Step 2: in the 1000ml there-necked flask that dropping funnel, thermometer, stirring are housed, add Sodium Glutamate 191g (1mol), be dissolved in 695.4g Virahol and water mixed solution (m Virahol: m water=1:5), stirring at normal temperature makes it dissolve, cocounut oil acyl chlorides is put into the dropping funnel of 500ml, water at low temperature bath temperature control is at 20 ~ 25 DEG C, under agitation add cocounut oil acyl chlorides 359g (1.2mol), drip the aqueous sodium hydroxide solution of 40% simultaneously, reacting liquid pH value is made to maintain pH=10 ~ 12, drip and finish, continue to stir 1h; After end, rise to room temperature, decompression desolventizing 1h; Cooling, temperature control, at 15 ~ 20 DEG C, drips hydrochloric acid under stirring, makes system pH=2 ~ 4, the crystallization of precipitate particle shape, suction filtration, after oven dry, obtains cocoyl L-glutamic acid 339g, yield 91%.
Embodiment 7
Step one: in the 500ml there-necked flask that stirrer, thermometer, airway, reflux condensing tube are housed,
Add coconut oil 284g (1mol) successively, N, N-N,N-DIMETHYLACETAMIDE 6.1g (0.07mol), is warming up to 70 DEG C, and controlling temperature of reaction is 70 ~ 75 DEG C, pass into phosgene 110g (1.1mol), react complete in 5 ~ 8 hours, reduced vacuum is distilled, and collects 140 ~ 180 DEG C of (560Pa) cuts, obtain cocounut oil acyl chlorides 265g, yield 88%.
Step 2: in the 1000ml there-necked flask that dropping funnel, thermometer, stirring are housed, add Sodium Glutamate 191g (1mol), be dissolved in the 572.2g trimethyl carbinol and water mixed solution (the m trimethyl carbinol: m water=1:3), stirring at normal temperature makes it dissolve, cocounut oil acyl chlorides is put into the dropping funnel of 500ml, water at low temperature bath temperature control is at 20 ~ 25 DEG C, under agitation add cocounut oil acyl chlorides 359g (1.2mol), drip the aqueous sodium hydroxide solution of 40% simultaneously, reacting liquid pH value is made to maintain pH=10 ~ 12, drip and finish, continue to stir 1h; After end, rise to room temperature, decompression desolventizing 1h; Cooling, temperature control, at 15 ~ 20 DEG C, drips hydrochloric acid under stirring, makes system pH=2 ~ 4, the crystallization of precipitate particle shape, suction filtration, after oven dry, obtains cocoyl L-glutamic acid 339g, yield 89%.
Claims (3)
1. a preparation method for cocoyl L-glutamic acid, is characterized in that, comprises step,
With coconut oil photoreactive gas for raw material, be 1:1.05 ~ 3.5:0.05 ~ 0.2 by the mol ratio of coconut oil, phosgene and catalyzer, under organic amine catalyst effect, coconut oil leads to phosgene reaction 5 ~ 30 hours under 70 ~ 120 DEG C of micro-molten states, react complete, reduced vacuum distillation obtains described cocounut oil acyl chlorides;
Under room temperature, be dissolved in by Sodium Glutamate in the mixing solutions of alcohol and water, the mass ratio of alcohol and water is 1:1.0 ~ 10.0, after dissolving, hierarchy of control temperature is 0 ~ 50 DEG C, under insulated and stirred, drip the aqueous solution of cocounut oil acyl chlorides and sodium hydroxide, the mol ratio of amino acid sodium and cocounut oil acyl chlorides is 1:1.0 ~ 1.6 simultaneously, about 0.5 ~ 6 hour, sodium hydroxide rate of addition and consumption maintain between 6 ~ 15 with system pH, drip and finish, stir 0.5 ~ 6h; At maintaining the temperature at 0 ~ 100 DEG C, decompression desolventizing 0.5 ~ 6h; Cooling, temperature control, at 0 ~ 50 DEG C, under agitation, slowly drips hydrochloric acid, and the amount that hydrochloric acid drips maintains between 0 ~ 10 with system pH, and drip and finish, the crystallization of precipitate particle shape, suction filtration, after oven dry, obtains cocoyl L-glutamic acid.
2. the preparation method of a kind of cocoyl L-glutamic acid according to claim 1, is characterized in that, described organic amide catalyzer is N; dinethylformamide, N,N-dimethylacetamide, pyridine or N, N-amide dimethyl butyrate; preferred catalyzer is DMF.
3. the preparation method of a kind of cocoyl L-glutamic acid according to claim 1; it is characterized in that; select alcohol and water mixing solutions to be solvent, described alcohol is the alcohols such as methyl alcohol, ethanol, propyl alcohol, Virahol, the trimethyl carbinol, isopropylcarbinol, and preferred alcohols is ethanol and Virahol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510945430.5A CN105541652A (en) | 2015-12-17 | 2015-12-17 | Preparation method of cocoyl glutamate acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510945430.5A CN105541652A (en) | 2015-12-17 | 2015-12-17 | Preparation method of cocoyl glutamate acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105541652A true CN105541652A (en) | 2016-05-04 |
Family
ID=55821270
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510945430.5A Pending CN105541652A (en) | 2015-12-17 | 2015-12-17 | Preparation method of cocoyl glutamate acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105541652A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106076191A (en) * | 2016-06-06 | 2016-11-09 | 大连民族大学 | A kind of anionic surfactant utilizing monosodium glutamate to prepare and preparation method thereof |
| CN110668965A (en) * | 2019-10-23 | 2020-01-10 | 铜仁学院 | Preparation method of cocoyl glutamic acid |
| CN110668964A (en) * | 2019-10-23 | 2020-01-10 | 铜仁学院 | Synthesis and preparation method of lauroyl glutamic acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61216724A (en) * | 1985-03-22 | 1986-09-26 | Kawaken Fine Chem Co Ltd | Preparation of n-long chain acylamino acid type surfactant and liquid detergent composition containing said surfactant |
| CN102863352A (en) * | 2012-09-05 | 2013-01-09 | 长沙普济生物科技有限公司 | Synthesizing method of cocoyl amino acid sodium |
| CN103505375A (en) * | 2012-06-22 | 2014-01-15 | 花王株式会社 | Liquid detergent composition |
-
2015
- 2015-12-17 CN CN201510945430.5A patent/CN105541652A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61216724A (en) * | 1985-03-22 | 1986-09-26 | Kawaken Fine Chem Co Ltd | Preparation of n-long chain acylamino acid type surfactant and liquid detergent composition containing said surfactant |
| CN103505375A (en) * | 2012-06-22 | 2014-01-15 | 花王株式会社 | Liquid detergent composition |
| CN102863352A (en) * | 2012-09-05 | 2013-01-09 | 长沙普济生物科技有限公司 | Synthesizing method of cocoyl amino acid sodium |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106076191A (en) * | 2016-06-06 | 2016-11-09 | 大连民族大学 | A kind of anionic surfactant utilizing monosodium glutamate to prepare and preparation method thereof |
| CN110668965A (en) * | 2019-10-23 | 2020-01-10 | 铜仁学院 | Preparation method of cocoyl glutamic acid |
| CN110668964A (en) * | 2019-10-23 | 2020-01-10 | 铜仁学院 | Synthesis and preparation method of lauroyl glutamic acid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105152957B (en) | The synthetic method of laurel acyl amino acid sodium | |
| EP2888226B1 (en) | Method to produce n-acyl amino acid surfactants using n-acyl amino acid surfactants or the corresponding anhydrides as catalysts | |
| CN102875409A (en) | Synthetic method of laurel acyl amino acid sodium | |
| CN102863348B (en) | A kind of synthetic method of palmitoyl amino acid sodium | |
| CN102863352A (en) | Synthesizing method of cocoyl amino acid sodium | |
| CN102276663B (en) | Preparation method of glucosamine sulfate | |
| CN102898382B (en) | Method for synthesizing 2-amino-4,6-dimethoxypyrimidine | |
| CN105541652A (en) | Preparation method of cocoyl glutamate acid | |
| CN102911086A (en) | Preparation method of trifluoro methanesulfonic anhydride | |
| CN111004156A (en) | Method for synthesizing fatty acyl amino acid surfactant by direct method | |
| CN103274959A (en) | Synthetic method of cooling agent N-, 2, 3-trimethyl-2-isopropyl butyrylamide | |
| CN104193636A (en) | Method for preparing beta-aminopropanoic acid ampholytic surfactant | |
| CN106831421A (en) | The preparation method of di-tert-butyl dicarbonate | |
| CN105254575A (en) | Synthetic method for sulfadiazine | |
| CN105884638A (en) | Alpha-lauryl betaine type dimeric surfactant and synthesis method thereof | |
| KR100974608B1 (en) | Method of producing 3-o-alkyl-5,6-o-1-methylethylidene-l-ascorbic acid and method of producing 5,6-o-1-methylethylidene-l-ascorbic acid | |
| CN104672127B (en) | 3,5,6-trichlopyr and the preparation method of salt thereof | |
| CN109761836A (en) | The preparation method of amides compound | |
| CN111333531B (en) | Preparation process of lauroyl sarcosine sodium and application of lauroyl sarcosine sodium in daily chemical field | |
| CN105001111A (en) | Preparation method of N-lauroyl-L-alanine saline solution with low inorganic salt content | |
| CN103864773B (en) | Razaxaban and its preparation method of intermediate | |
| CN102875422A (en) | New synthesis method of N-acyl-N-methyltaurine | |
| CN103012473B (en) | A kind of synthetic method of pmida98 | |
| CN110117234B (en) | Synthesis method of N-fatty acyl glutamic acid alkali metal salt | |
| CN101575301B (en) | Preparation method of 2-amino-5-chlorobenzamide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160504 |
|
| RJ01 | Rejection of invention patent application after publication |