CN207793119U - The device of continuous production high-quality N- fatty acyl amino-acid salt surfactants - Google Patents

The device of continuous production high-quality N- fatty acyl amino-acid salt surfactants Download PDF

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CN207793119U
CN207793119U CN201721842777.8U CN201721842777U CN207793119U CN 207793119 U CN207793119 U CN 207793119U CN 201721842777 U CN201721842777 U CN 201721842777U CN 207793119 U CN207793119 U CN 207793119U
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entrance
amidation
column
mixing arrangement
acid salt
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方银军
徐坤华
葛赞
王晓辉
华文高
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Zhejiang Yabrown Technology Co ltd
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Jiaxing Zanyu Technology Co Ltd
Praise Technology Group Ltd By Share Ltd
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Abstract

The utility model belongs to daily-use chemical industry technical field.Purpose is to provide a kind of concise in technology, the device of the remaining continuous production high-quality N fatty acyls amino-acid salt surfactant of organic solvent-free.It is remained using the N fatty acyl amino-acid salt organic solvent-frees that the device produces, and can effectively improve the conversion ratio of acyl chlorides, reduce the content of sodium soap, improve product quality.Technical solution is:A kind of device of continuous production high-quality N fatty acyl amino-acid salt surfactants, it is characterised in that:Mixing arrangement, heat exchanger and the amidation column that the device is sequentially communicated including the use of pipeline, are then divided into two-way, are respectively connected to the second entrance of mixing arrangement and connect aging device entrance by heater, the aging device is equipped with products export;The first entrance of the mixing arrangement connects ispol entrance parallel with one another, acyl chlorides entrance and liquid caustic soda entrance.

Description

The device of continuous production high-quality N- fatty acyl amino-acid salt surfactants
Technical field
The utility model belongs to daily-use chemical industry technical field, specifically continuous production high-quality N- fat acylamino-s The device of acid salt surfactant.
Background technology
Surfactant is however big at present due to unique application performance, being concerned and applying in numerous areas Most surfactants belong to petroleum-based sources, due to raw material non-renewable, low chemical safety and refractory organics and It receives and denounces.
With the continuous development of industrial technology, novel surfactant is come out one after another, and amino acid surfactant is exactly it In one kind.Due to raw material natural reproducible and its own with excellent surface-active, good calcium soap dispersibility, it is excellent The advantages such as different bacteriostasis, high security, low irritant, easily biological-degradable and good Environmental compatibility, amino acid surface Activating agent obtains in fields such as daily use chemicals, food, beverage, bio-pharmaceuticals, mineral floating, metal cleaner, textile printing and dyeing, agriculture breasts Relatively broad research and application.External manufacturing firm has the Hamposyl series of Dow company, Switzerland's Clariant public Medialan and the Hostapon series of department, the Amisoft series of Japanese aginomoto;There are lion in Nanjing, Guangzhou in domestic producer Be bestowed by heaven, profit is inspired confidence in Guangzhou hundred, Shanghai profit contain etc..
The production of amino acid surfactant has enzyme-catalyzed change method, such as Hasmah Bidin have studied through lipase RM IM is catalyzed palm grease and lysine prepares amino acid surfactant;Also dehydrating condensation method, such as Woodbury have studied Under hot conditions, aliphatic acid can directly generate corresponding amino acid surfactant with amino acid alkali metal salt.But due to various Reason, the industrialized production of amino acid surfactant is main at present or indirect method --- chemical synthesis, such as patent CN 104640839B is disclosed according to Schotten- Baumann condensation method principles, using N- acyl amino acid surfactants or Corresponding acid anhydrides produces N- acyl amino acid surfactants as catalyst;Patent JP11180938 is condensation with water-tert-butyl alcohol Reaction dissolvent forms stable water/tert-butyl alcohol/active matter ternary system and again secondary clearing, then obtains product by distilation; US20150126776 uses glycerine as solvent, and alkali or alkaline earth metal oxide, alkali metal methoxide etc. are as catalysis Agent synthesizes N- fatty acyl amino-acid salts;Patent WO2015026538 better products of color and luster in order to obtain, use methanol as solvent. Patent CN102311359A and CN105439882A disclose a kind of fatty instead of fat acyl chloride synthesis N- using fatty acid methyl ester The method of acyl amino acids surfactant.
In existing research and patent document, many improvement and wound have been carried out to the preparation of amino acid surfactant Newly, it is still current main industrialized production that acyl chlorides is reacted with amino acid condensation.In order to improve reaction conversion ratio and N- The yield of fatty acid acylamino acid class surfactant needs in technique productions methanol, the tert-butyl alcohol, glycerine etc. is added organic molten Agent;And although the organic solvent being added have passed through the removing of subsequent technique, but inevitably still have part residual, to product Quality, using exerting a certain influence.
Utility model content
The purpose of the utility model is to overcome the deficiencies of above-mentioned technology, provide a kind of concise in technology, organic solvent-free residual Continuous production high-quality N- fatty acyl amino-acid salt surfactants device.The N- fatty acyl ammonia produced using the device Base hydrochlorate organic solvent-free remains, and can effectively improve the conversion ratio of acyl chlorides, reduces the content of sodium soap, improves product Quality.
The technical solution of the utility model is:
A kind of device of continuous production high-quality N- fatty acyl amino-acid salt surfactants, it is characterised in that:The dress Mixing arrangement, heat exchanger and the amidation column being sequentially communicated including the use of pipeline are set, is then divided into two-way, is respectively connected to mix The second entrance of device and by heater connect aging device entrance, the aging device be equipped with products export;The mixing dress The first entrance set connects ispol entrance parallel with one another, acyl chlorides entrance and liquid caustic soda entrance.
The amidation column is the overflow column with stirring, and arrival end is located at amidation column bottom, and outlet end is located at amide Change column upper side.
The mixing arrangement includes static mixer or shear pump.
The aging device is the column reactor suitable for successive reaction, or is the still reaction suitable for intermittent reaction Device.
Compared with prior art, the utility model has the advantage that:
(1) it in existing N- fatty acyls amido hydrochlorate production technology, needs to add organic solvent, and the utility model does not need Add organic solvent;So as to avoid in product the problem of organic solvent residual.
(2) solvent production N- fatty acyl amino-acid salts are used water as, reaction system needs to maintain higher pH, but with The progress of reaction, pH are drastically reduced, and are unfavorable for the progress of amidation process, but the decomposition of side reaction acyl chlorides increases Add, generate a large amount of sodium soap, influences product quality and performance;The utility model technique uses the amino acid of different isoelectric points It is compounded, has obtained, with the reaction system for stablizing buffer pH, to keep reacting required higher pH, while can effectively inhibit The decomposition of acyl chlorides considerably reduces the generation of sodium soap, and 80% can be about reduced compared with unitary system sodium soap.
(3) water law is utilized to produce N- fatty acyl amino-acid salts, with the progress of reaction, amino acid and acyl chlorides persistently disappear Consumption, can lead to the continuous decrease of pH value of reaction system, need to continue to mend alkali in conventional production and maintain optimum response pH value, therefore compared with Hardly possible realizes the continuous production of the technique.The utility model technique is compounded using the amino acid of different isoelectric points, is had There is the raw material reaction system that pH bufferings are adjusted;The reaction simultaneously is flowed back using ratio, and amidation process material is fully mixed with virgin material It closes, amidation process pH is made to obtain stability contorting;The two collective effect, during effectively can controlling continuous reaction, pH value Always in best pH value in reaction;Enable continuous production is simple smoothly to implement.
(4) each device in the utility model is conventional components, thus technology maturation, service life are long, and cost is not yet It is high.
Description of the drawings
Fig. 1 is the knot of continuous production high-quality N- fatty acyls amino-acid salt surfactant device described in the utility model Structure schematic diagram.
Wherein:A is ispol entrance, and b is acyl chlorides entrance, and c is liquid caustic soda entrance, and d is products export, and 1 is mixing Device, 2 be heat exchanger, and 3 be delivery pump, and 4 be amidation column, and 5 be heater, and 6 be aging device.
Specific implementation mode
The utility model is compounded amino acid starting material reaction system, can effectively adjust required soda acid ring in reaction process Border, be it is a kind of it is completely new, suitable for the preparation system of industrialized production high-quality N- fatty acyl amino-acid salts.
A kind of device of continuous production high-quality N- fatty acyl amino-acid salt surfactants, successively including the use of pipeline Mixing arrangement 1, heat exchanger 2 and the amidation column 4 of connection, are then divided into two-way, are respectively connected to the second entrance of mixing arrangement And aging device entrance is connected by heater 5, the aging device is equipped with products export;The first entrance of the mixing arrangement connects Logical ispol entrance a, acyl chlorides entrance b and liquid caustic soda entrance c parallel with one another.
The amidation column is the overflow column with stirring, and arrival end is located at amidation column bottom, and outlet end is located at amide Change column upper side.
The mixing arrangement includes static mixer or shear pump.
The aging device is the column reactor suitable for successive reaction, or is the still reaction suitable for intermittent reaction Device.
Using the technique of above-mentioned apparatus continuous production high-quality N- fatty acyl amino-acid salt surfactants, including it is following Step:
(1) it is mixed to respectively enter a mixing arrangement for reaction mass ispol, acyl chlorides, liquid caustic soda and circulating and recovering material It is even;
(2) material after mixing enters one by bottom using a delivery pump and carries overflow port after heat exchanger cools down In amidation column, amidation process is carried out under suitable temperature, pH value;
(3) product after amidation through amidation column overflow port spilling after, a part be used as circulating and recovering material, again into Enter mixing arrangement and carries out circular response;After the heated device heating of another part, aging reaction is carried out into aging device;The cycle The mass ratio of reuse material and the material for entering aging device is 2-20:1;
(4) reaction product after aging, that is, object N- fatty acyl amino-acid salts;
Ispol is the aqueous solution or/and amino-acid salt mixture of ispol in the step (1) Aqueous solution;The mass concentration of aqueous solution is 5-50%;It is preferred that 10-30%.
The ispol is two amino acids and its saline admixture, one type include isoelectric point 7.0 with Under amino acid and its esters one or more;Another kind of includes amino acid and its esters of the isoelectric point 9.0 or more It is one or more kinds of;The mass ratio of two amino acids and its saline admixture is 100:1-20.
The isoelectric point is glycine, alanine or glutamic acid in 7.0 amino acid below;The isoelectric point 9.0 with On amino acid be lysine or arginine.
The reaction mass ispol, acyl chlorides, liquid caustic soda and circulating and recovering material pan feeding flow by amidation The dischargeable capacity of column determines;It is 2-24h, preferably 4- to generally require mean residence time of the control material in amidation column 10h;
The mass ratio of the pan feeding substance of the ispol and acyl chlorides is 1.0~3.0:1;The liquid caustic soda flow according to PH value into amidation pre-column reaction system determines;The pH value into amidation pre-column reaction system is 7-12, preferably For 8-11;The liquid caustic soda flow is automatically controlled by the way that online pH meter is chain, or is manual adjusting control;
The acyl chlorides is the fatty acid chloride of C8-C18, preferably lauroyl chloride, cocounut oil acyl chlorides, palmitoyl chloride;The liquid caustic soda Mass concentration be 5-50%, preferably 10-32%;
Suitable reaction temperature described in step (2) is 5-50 DEG C, preferably 10-30 DEG C.
Aging temperature described in step (3) be 20-100 DEG C, preferably 40-80 DEG C, ageing time 2-24h, preferably 4- 12h。
The utility model is further illustrated below in conjunction with specific embodiment.
Embodiment 1:Ispol aqueous solution (the wherein mass ratio of alanine and lysine that mass concentration is 20% It is 100:8), lauroyl chloride, the liquid caustic soda that mass concentration is 20% respectively enter mixing arrangement and are uniformly mixed, and wherein amino acid mixes The charging rate of the charging rate 108kg/h of object aqueous solution, lauroyl chloride are 40kg/h, and the flow of liquid caustic soda is read according to pH meter Automatic adjustment controls pH9.5 ± 0.2;The speed of circular response material is 1000kg/h;After cooler cools down, conveying is utilized Pump, which is transported in amidation column, carries out amidation process, 20 DEG C of controlling reaction temperature, stop of the reaction mass in amidation column Time is 5h;Product after reaction enters aging kettle by 200kg/h, and control aging temperature is 60 DEG C, ageing time 6h;Remaining Product after reaction enters mixing arrangement as recycle stock and continues to react.
Embodiment 2:Ispol aqueous solution (the wherein mass ratio of alanine and lysine that mass concentration is 25% It is 100:10), cocounut oil acyl chlorides, the liquid caustic soda that mass concentration is 15% respectively enter mixing arrangement and are uniformly mixed, and wherein amino acid is mixed The charging rate 50kg/h of object aqueous solution is closed, the charging rate of acyl chlorides is 36kg/h, and the flow of liquid caustic soda is read automatically according to pH meter It adjusts, controls pH10.0 ± 0.2;The speed of circular response material is 1000kg/h;After cooler cools down, delivery pump is utilized It is transported in amidation column and carries out amidation process, 18 DEG C of controlling reaction temperature, when stop of the reaction mass in amidation column Between be 6h;Product after reaction enters aging kettle by 160kg/h, and control aging temperature is 70 DEG C, ageing time 4h;Remaining Product after reaction enters mixing arrangement as recycle stock and continues to react.
Embodiment 3:Ispol aqueous solution (the wherein alanine and arginic mass ratio that mass concentration is 15% It is 100:2), lauroyl chloride, the liquid caustic soda that mass concentration is 32% respectively enter mixing arrangement and are uniformly mixed, and wherein amino acid mixes The charging rate of the charging rate 152kg/h of object aqueous solution, acyl chlorides are 50kg/h, and the flow of liquid caustic soda reads automatic adjust according to pH meter Section controls pH10.5 ± 0.2;The speed of circular response material is 1000kg/h;It is defeated using delivery pump after cooler cools down It is sent in amidation column and carries out amidation process, 15 DEG C of controlling reaction temperature, residence time of the reaction mass in amidation column For 4h;Product after reaction enters aging kettle by 250kg/h, and control aging temperature is 50 DEG C, ageing time 8h;Remaining reaction Product afterwards enters mixing arrangement device as recycle stock and continues to react.
Embodiment 4:Ispol aqueous solution (the wherein alanine and arginic mass ratio that mass concentration is 30% It is 100:1), cocounut oil acyl chlorides, the liquid caustic soda that mass concentration is 15% respectively enter mixing arrangement and are uniformly mixed, and wherein amino acid mixes The charging rate of object aqueous solution is 48kg/h, and the charging rate of acyl chlorides is 38kg/h, and the speed of circular response material is 1000kg/ h;The flow of liquid caustic soda reads according to pH meter and automatically adjusts, and controls pH10.0 ± 0.2;It is defeated using delivery pump after cooler cools down It is sent in amidation column and carries out amidation process, control amidation process temperature is 18 DEG C;Reaction mass is in amidation column Residence time is 6h;Product after reaction enters aging kettle by 150kg/h, and control aging temperature is 65 DEG C, ageing time 6h; Product after remaining reaction enters mixing arrangement as recycle stock and continues to react.
Comparative example 1:The liquid caustic soda that the third amino acid solution that mass concentration is 20%, lauroyl chloride, mass concentration are 20% It respectively enters mixing arrangement to be uniformly mixed, wherein the charging rate 88kg/h of alanine aqueous solution, the charging rate of acyl chlorides are 36kg/h, the flow of liquid caustic soda is read according to pH meter to be automatically adjusted, and pH10.0 ± 0.2 is controlled;The speed of circular response material is 1000kg/h;After cooler cools down, it is transported in amidation column using delivery pump and carries out amidation process, controlling reaction temperature 20 DEG C, residence time of the reaction mass in amidation column is 5h;Product after reaction enters aging kettle by 200kg/h, enters It is 60 DEG C to control aging temperature, ageing time 6h;Product after remaining reaction enters mixing arrangement as recycle stock to be continued It is reacted.
Comparative example 2:The liquid caustic soda that bad amino acid solution that mass concentration is 20%, cocounut oil acyl chlorides, mass concentration are 32% Mixing arrangement mixing, wherein the charging rate 76kg/h of lysine solution are respectively enterd, the charging rate of acyl chlorides is 30kg/h, The flow of liquid caustic soda reads according to pH meter and automatically adjusts, and controls pH10.5 ± 0.2;The speed of circular response material is 1000kg/h; After cooler cools down, it is transported in amidation column using delivery pump and carries out amidation process, 20 DEG C of controlling reaction temperature, reaction Residence time of the material in amidation column is 6h;Product after reaction enters aging kettle by 150kg/h, into control aging temperature Degree is 60 DEG C, ageing time 8h;Product after remaining reaction enters mixing arrangement as recycle stock and continues to react.
1 product test data comparison of table
Index Appearance Color and luster, Hazen Sodium soap, %
Embodiment 1 Clear 10 0.9
Embodiment 2 Clear 12 1.1
Embodiment 3 Clear 13 1.1
Embodiment 4 Clear 10 0.8
Comparative example 1 Clear 30 5.4
Comparative example 2 Clear 28 5.8
PH value changes before and after 2 amidation of table
Index PH before column PH after column
Embodiment 1 9.7 9.4
Embodiment 2 10.1 9.7
Embodiment 3 10.6 10.1
Embodiment 4 10.1 9.6
Comparative example 1 10.2 8.1
Comparative example 2 10.5 8.3
It was found from test data:The color and luster of 4 embodiments is significantly better than comparative example, the sodium soap content of 4 embodiments Then it is considerably less than comparative example.Obtain satisfactory effect.

Claims (2)

1. a kind of device of continuous production high-quality N- fatty acyl amino-acid salt surfactants, it is characterised in that:The device Mixing arrangement (1), heat exchanger (2) and the amidation column (4) being sequentially communicated including the use of pipeline, are then divided into two-way, respectively It accesses the second entrance of mixing arrangement and (5) is connected by heater and connect aging device entrance, the aging device is equipped with products export; The first entrance of the mixing arrangement is connected ispol entrance (a) parallel with one another, acyl chlorides entrance (b) and liquid caustic soda and is entered Mouth (c);
The amidation column is the overflow column with stirring, and arrival end is located at amidation column bottom, and outlet end is located at amidation column Upper side.
2. the device of continuous production high-quality N- fatty acyl amino-acid salt surfactants according to claim 1, It is characterized in that:The mixing arrangement includes static mixer or shear pump;The aging device is the pillar suitable for successive reaction Reactor, or be the tank reactor suitable for intermittent reaction.
CN201721842777.8U 2017-12-26 2017-12-26 The device of continuous production high-quality N- fatty acyl amino-acid salt surfactants Active CN207793119U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108003050A (en) * 2017-12-26 2018-05-08 赞宇科技集团股份有限公司 A kind of technique and device of continuous production high-quality N- fatty acyl amino-acid salt surfactants
CN115504898A (en) * 2022-09-22 2022-12-23 山东万盛新材料有限公司 Preparation method of N-acyl acidic amino acid alkali metal salt aqueous solution

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108003050A (en) * 2017-12-26 2018-05-08 赞宇科技集团股份有限公司 A kind of technique and device of continuous production high-quality N- fatty acyl amino-acid salt surfactants
CN108003050B (en) * 2017-12-26 2024-03-08 赞宇科技集团股份有限公司 Process and device for continuously producing high-quality N-fatty acyl amino acid salt surfactant
CN115504898A (en) * 2022-09-22 2022-12-23 山东万盛新材料有限公司 Preparation method of N-acyl acidic amino acid alkali metal salt aqueous solution

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Effective date of registration: 20240313

Address after: B1-3-231, No. 198 Qidi Road, Economic and Technological Development Zone, Xiaoshan District, Hangzhou City, Zhejiang Province, 311200

Patentee after: Zhejiang Yabrown Technology Co.,Ltd.

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Address before: Hangzhou City, Zhejiang province 310009 City Shangcheng District No. 128 Lane

Patentee before: ZANYU TECHNOLOGY GROUP CO.,LTD.

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Patentee before: JIAXING ZANYU TECHNOLOGY DEVELOPMENT Co.,Ltd.