CN103242206A - Production process for preparing fatty acyl-N-sodium methyl taurate surfactant - Google Patents
Production process for preparing fatty acyl-N-sodium methyl taurate surfactant Download PDFInfo
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- CN103242206A CN103242206A CN2013102089570A CN201310208957A CN103242206A CN 103242206 A CN103242206 A CN 103242206A CN 2013102089570 A CN2013102089570 A CN 2013102089570A CN 201310208957 A CN201310208957 A CN 201310208957A CN 103242206 A CN103242206 A CN 103242206A
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Abstract
The invention discloses a production process for preparing a fatty acyl-N-sodium methyl taurate surfactant. Single-kettle operation is changed into double-kettle operation in the production process. The production process comprises the following steps of: firstly, adding an N-sodium methyl taurate aqueous solution into a condensation reaction kettle, then, cooling the N-sodium methyl taurate aqueous solution, and changing the tail end of a fatty acyl chloride feeding pipe into a liquid drop spraying device, wherein the spraying device is provided with small holes, feed liquid is sprayed out of the small holes under the action of pressure and dispersed into fine liquid drops under the conditions of different-angle spray and mutual collision, fatty acyl chloride is dropped on the surface of the reaction feed liquid in a fine liquid drop way in the reaction process, and meanwhile, a catalyst and an acid-binding agent are dropwise added; and after the feeding operation is ended, transferring a rough product to an emulsifying kettle, gradually heating materials, enabling the residual fatty acyl chloride to completely react, meanwhile, defoaming and sterilizing, and adjusting the pH value. The production process has the advantages that the production time for producing a batch of products can be shortened by over 50%, so that the production efficiency is greatly increased; and meanwhile, the equipment is simple and easy to operate, and the quality of the product is easy to control.
Description
Technical field
The present invention relates to the field of chemical synthesis, relate in particular to a kind of production technique for preparing fatty acyl group-N methyl taurine natrium surfactant.
Background technology
The long acyl amino acid type surfactant since advantages such as its extremely low pungency, nontoxic, readily biodegradable obtained using widely.Fatty acyl group-N methyl taurine sodium belongs to a class of long acyl amino acid type surfactant; in molecule, has the sulfonic group of being combined with amide group; with negatively charged ion; nonionic; amphoterics has good compatibility; it is the higher anion surfactant of a kind of security; have good water-soluble; stability in hard water; alkali resistance; acid resistance; foaminess is also very good; feel after washing is fine; can give hair; the skin gentleness; moisten; smooth sensation; adapt to all kinds of medium-to-high grade shampoos of preparation; cleansing milk and bathe agent also can be used as the refining agent of wool spinning and silk printing and dyeing industry; detergent.Fatty acyl group-N methyl taurine natrium surfactant generally can be made by direct method and indirect method; direct method refers to that the technology of carrying out condensation reaction with lipid acid or fatty acid ester (vegetable and animals oils) and N methyl taurine sodium, indirect method synthesis technique then mainly are fatty nitrile hydrolysis acylation reaction technology, fat acyl chloride and N methyl taurine sodium at the Xiao Dun-Bao Man reaction process of basic catalyst effect etc.
It is raw material with lipid acid (as stearic acid, coconut oil) that US Patent No. 5496959A provides a kind of, directly and the technology of N methyl taurine sodium condensation prepared fatty acyl group-N methyl taurine sodium.At present direct method is because problem such as its reaction yield is low, severe reaction conditions and having difficulties in industrialization, at present at the industrial main Xiao Dun-Bao Man condensation process that adopts indirect method.
Technology with Xiao Dun-Bao Man condensation production fatty acyl group-N methyl taurine natrium surfactant mainly is divided into single pot of production and single pot of batch production continuously at present.Produce continuously for single pot and have the high advantage of level of automation; but needing earlier, prefabricated a certain amount of finished product circulates; the equipment manufacturing cost height; require high at start-stop car and maintenance of the equipment; be fit to the relatively low Xiao Dun-Bao Man condensation reaction of fat acyl chloride hydrolytic activity in the very big and synthesis material of demand to finished product, as with the oleoyl chloride being raw material synthetic oil acyl group N-methyltaurine sodium (209 washing composition).Because Xiao Dun-Bao Man reaction is to carry out under alkaline condition; this will speed up the hydrolysis of fat acyl chloride; document " the synthetic and performance of cocoyl N-methyltaurine sodium "; the household chemicals science; 2009,6, adopt single pot of method to synthesize cocoyl N-methyltaurine sodium; optimizing under the technology, the percent hydrolysis of cocounut oil acyl chlorides is more than 7%.For reducing the percent hydrolysis of fat acyl chloride in Xiao Dun-Bao Man reaction, the measure that can take in the production mainly contains the amount of substance ratio that reduces temperature of reaction, increase raw material N methyl taurine sodium and fat acyl chloride, three aspects of dispersion efficiency that improve fat acyl chloride.For the measure that reduces temperature of reaction, the hydrolysis that suppresses fat acyl chloride there is certain effect, but also can reduces the speed of main reaction simultaneously, can consume too much energy on the one hand, also can extend manufacture cycle on the other hand.Improve the feed ratio of N methyl taurine sodium, the generation of minimizing side reaction that can be to a certain degree under its excessive situation suppresses the effect of acyl chlorides hydrolysis and not obvious but surpass back to a certain degree, and is irrational in production cost control.The dispersion efficiency that improves fat acyl chloride is improvement and the innovation direction with this explained hereafter fatty acyl group-N methyl taurine sodium product.
US Patent No. 6828452 has been announced a kind of improved pair of dropping equipment, carry out material circulation and heat exchange by external on a reactor refrigeration switching equipment, play the effect that reduces temperature of charge and disperse fat acyl chloride, be fit to the production technique that the multiple fat acyl chloride of preparation and amino acid condensation prepare tensio-active agent.
Chinese patent CN102126984A has announced a kind of condensation production technique and specific equipment of N-long acyl amino acid salts; pass through external filler pre-mixing apparatus in this patent of invention; improved the velocity of diffusion of fat acyl chloride; thereby improve the quality of tensio-active agent; the content of soap in product has reduced 50%-75% than single pot of reaction; feed ratio reduces, and the condensation required time reduces.This invention feeds intake, the operations such as adjustment of blowing and pH value are mainly carried out in a reactor, still belongs to single pot of operation, the fat acyl chloride that adds reactive system before entering pre-mixing apparatus and premix still can be in excessive state before being reacted to a certain degree.
In sum, single pot of method of main employing is produced fatty acyl group-N methyl taurine natrium surfactant both at home and abroad at present, reducing the fat acyl chloride hydrolysis, improves the quality of products, and shortens on production cycle and the raising products production efficient still remaining to be improved.
In adopting single pot of traditional method production; the N methyl taurine sodium water solution adds in the reactor earlier; fat acyl chloride, basic catalyst and acid-binding agent add in the reactor in the mode of two droppings; we find the carrying out along with reaction; the excessive degree of N methyl taurine sodium reduces, and all has local excessive situation in fat acyl chloride adding reaction charge level or the reaction material, to the big operation of the fast or single batch of feed rate; the hydrolysis situation of acyl chlorides is more serious, has a strong impact on the quality of product.Relatively stricter to the conditional request of temperature controlling in producing and pH value simultaneously, product viscosity is higher, and the time of blowing packing is also long, and production efficiency is not high.
Summary of the invention
Technical problem solved by the invention is to provide a kind of production technique for preparing fatty acyl group-N methyl taurine natrium surfactant, to solve the problem in the above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
A kind of production technique for preparing fatty acyl group-N methyl taurine natrium surfactant, by single pot of operation being changed into two pot operations, in the condensation reaction still, add the N methyl taurine sodium water solution earlier, repack fat acyl chloride filling tube end into the drop flusher, flusher is elongate tubular or disc, be distributed with the aperture of diameter 0.2-2mm on the body of flusher or the card, under pressure, feed liquid sprays from aperture, under the injection of different angles and colliding mutually, feed liquid is dispersed into fine drop, in reaction process, fat acyl chloride is dropped in the reaction solution charge level in the mode of fine drop, improved dispersion efficiency greatly, avoided local excessive and the hydrolysis that causes has also improved feed rate simultaneously, shorten the reaction times, dripped catalyzer and acid binding agent simultaneously; After reinforced the finishing, thick transferred product is to the emulsification pot, and the temperature of charge that raises gradually reacts completely the fat acyl chloride of remnants, carries out froth breaking sterilization and the adjustment of pH value simultaneously.Viscosity reduces after the product liquefaction, and flowability improves, and the blowing package speed is accelerated, the operation simultaneously of two pots, and the production time of single batch of product can reduce more than 50%, has improved production efficiency greatly, the while device simple, simple to operate, quality product is controlled easily.
Adopt in the technology of the present invention, described fat acyl chloride is for being selected from cocounut oil acyl chlorides, lauroyl chloride, cardamom acyl chlorides, palmityl chloride, stearyl chloride, oleoyl chloride, C
8-24At least a in the fat acyl chloride, header tank is deposited, and drips pipeline and flusher is added dropwise in the acylation reaction still through acyl chlorides.Can select the pressure exerting device of assisting, increase the hydraulic pressure of acyl chlorides, so that the drop that sprays is evenly tiny.
Adopt in the technology of the present invention; the quality percentage composition of N methyl taurine sodium is 5%-80% in the described N methyl taurine sodium water solution, preferred 10%-60%, more preferably 15%-40%; before dripping the fat acyl chloride reaction, join in the reactor earlier and cool, up to the temperature of reaction of setting.To this technology, temperature of reaction should be controlled below 60 ℃, preferably controls below 40 ℃, more preferably controls below 30 ℃.The cooling of reactive system is by the external refrigeration equipment control of reactor.
Adopt in the technology of the present invention, described catalyzer and acid binding agent are for selecting NaOH, KOH, NaCO for use
3, KCO
3In at least a aqueous solution that is made into, header tank is deposited, and drips pipeline through catalyzer and be added dropwise in the acylation reaction still.To this technology, the pH value of condensation reaction should be controlled below 11.5, preferably controls below 10.5, more preferably should control below 10.
Adopt in the technology of the present invention, be added dropwise to complete the back material at fat acyl chloride and acid-binding agent and be transferred in the emulsification pot, by the external heating installation heating of emulsification pot, the temperature of charge that raises gradually, to material liquefaction, bubble is eliminated.To this technology, temperature of charge should be controlled below 100 ℃ in the emulsification pot, preferably controls below 90 ℃, more preferably controls below 80 ℃.
Adopt in the technology of the present invention, pH adjusts agent and can select for use organic acid also can select mineral acid for use, example hydrochloric acid, sulfuric acid, phosphoric acid, citric acid, tartrate, oxysuccinic acid, preferred hydrochloric acid.PH adjusts agent by header tank and drips pipeline and introduces in the emulsification pot, adjusts material pH value to required degree, and to this technology, material pH value should be transferred below 10, and is preferred below 9, more preferably below 8.
Compared with prior art, the invention has the beneficial effects as follows: the present invention can reduce more than 50% single batch of production time of producing product, has improved production efficiency greatly, the while device simple, and simple to operate, quality product is controlled easily.
Description of drawings
Fig. 1 is main technique and the schema of two pot explained hereafter fatty acyl groups-N methyl taurine natrium surfactant.
Fig. 2 is elongate tubular dropper vertical cross section.
Fig. 3 is disc dropper plumb cut figure.
Among Fig. 1,1-air compressor, 2-refrigerator, 3-acyl chlorides header tank, 4-catalyzer and acid-binding agent header tank, 5-condensation reaction still, the 6-flusher, 7-pump, 8-steam heater, the 9-header tank, 10-emulsification pot, 11-is to acyl chlorides header tank pipeline, and 12-is to the pump line road, 13-is to emulsification pan pipe road, 14-discharge pipe.
Among Fig. 2,21-body, 22-perforate, 23-end socket.
Among Fig. 3,31-card, 32-opening area.
Embodiment
In order to make technique means of the present invention, creation characteristic, workflow, using method reach purpose and effect is easy to understand, below further set forth the present invention.
Embodiment 1
With the two pot reaction production cocoyl-N methyl taurine sodium shown in the accompanying drawing 1, operating process is as follows: be that 40%N-N-methyltaurine sodium water solution 278kg adds in the reactor with massfraction, add deionized water 170kg.With 154kg cocounut oil acyl chlorides suction acyl chlorides header tank, the corresponding header tank of 100kg acid-binding agent suction.Start refrigerator, the aqueous solution with N methyl taurine sodium under stirring is cooled to 15 ℃, begins to drip acyl chlorides, catalyzer and acid-binding agent, and cocounut oil acyl chlorides rate of addition is controlled at 50-60L/h, and the acid-binding agent rate of addition is controlled at 35-40L/h.In dripping the material reaction process, the material temperature should be controlled below 40 ℃, and the pH value should be controlled between 9-11, and 3-3.5h dropwises, material is transferred to the emulsification pot, start steam heating, stir the material temperature that raises gradually down to 75 ℃, the feed liquid transparent flow is good, being added dropwise to massfraction from header tank is 31% concentrated hydrochloric acid 2kg, product pH value is transferred to 7.0-8.5, and sampling detects, the blowing packing.Parallel production is 16 batches under above-mentioned feed ratio and other operating procedure condition, and each batch data is as follows:
The mean value of two pot technologies of the present invention and former single pot of each index of method technology is compared as follows:
Embodiment 2
Produce lauroyl-N methyl taurine sodium with the two pot reactions shown in the accompanying drawing 1, operating process is as follows: be that 40%N-N-methyltaurine sodium water solution 275kg adds in the reactor with massfraction, add deionized water 170kg.With 155kg lauroyl chloride suction acyl chlorides header tank, the corresponding header tank of 100kg acid-binding agent suction.Start refrigerator, the aqueous solution with N methyl taurine sodium under stirring is cooled to 18 ℃, begins to drip acyl chlorides, catalyzer and acid-binding agent, and the lauroyl chloride rate of addition is controlled at 50-60L/h, and the acid-binding agent rate of addition is controlled at 35-40L/h.In dripping the material reaction process, the material temperature should be controlled below 45 ℃, and the pH value should be controlled between 9-11, and 3-3.5h dropwises, material is transferred to the emulsification pot, start steam heating, stir the material temperature that raises gradually down to 80 ℃, the feed liquid transparent flow is good, being added dropwise to massfraction from header tank is 31% concentrated hydrochloric acid 2kg, product pH value is transferred to 7.0-8.5, and sampling detects, the blowing packing.
Parallel production is 6 batches under above-mentioned feed ratio and other operating procedure condition, and each batch data is as follows:
The mean value of two pot technologies of the present invention and former single pot of each index of method technology is compared as follows:
Embodiment 3
With the acyl group-N methyl taurine sodium that produces oil of the two pot reactions shown in the accompanying drawing 1, operating process is as follows: be that 40%N-N-methyltaurine sodium water solution 205kg adds in the reactor with massfraction, add deionized water 320kg.With 115kg oleoyl chloride suction acyl chlorides header tank, the corresponding header tank of 66kg acid-binding agent suction.Start refrigerator, the aqueous solution with N methyl taurine sodium under stirring is cooled to 20 ℃, begins to drip acyl chlorides, catalyzer and acid-binding agent, and the oleoyl chloride rate of addition is controlled at 50-60L/h, and the acid-binding agent rate of addition is controlled at 35-40L/h.In dripping the material reaction process, the material temperature should be controlled below 60 ℃, and the pH value should be controlled between 9-11, and 3-3.5h dropwises, material is transferred to the emulsification pot, start steam heating, stir the material temperature that raises gradually down to 85 ℃, the feed liquid transparent flow is good, being added dropwise to massfraction from header tank is 31% concentrated hydrochloric acid 1.2kg, product pH value is transferred to 7.0-8.5, and sampling detects, the blowing packing.
Parallel production is 6 batches under above-mentioned feed ratio and other operating procedure condition, and each batch data is as follows:
The mean value of two pot technologies of the present invention and former single pot of each index of method technology is compared as follows:
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and the specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (10)
1. production technique for preparing fatty acyl group-N methyl taurine natrium surfactant, it is characterized in that, change single pot of operation into two pot operations, in the condensation reaction still, add the N methyl taurine sodium water solution earlier, the quality percentage composition of N methyl taurine sodium is 5%-80% in the described N methyl taurine sodium water solution, cool again, temperature of reaction control is below 60 ℃, repack fat acyl chloride filling tube end into the drop flusher, flusher is provided with aperture, and under pressure, feed liquid sprays from aperture, under the injection of different angles and colliding mutually, feed liquid is dispersed into fine drop, and in reaction process, fat acyl chloride is dropped in the reaction solution charge level in the mode of fine drop, drip catalyzer and acid binding agent simultaneously, the pH value control of condensation reaction is below 11.5; After reinforced the finishing, to the emulsification pot, raise gradually temperature of charge and control is below 100 ℃ with thick transferred product, and the fat acyl chloride of remnants is reacted completely, and carries out the froth breaking sterilization simultaneously, adjusts agent with pH and adjusts the pH value below 10.
2. the production technique of preparation fatty acyl group according to claim 1-N methyl taurine natrium surfactant is characterized in that, described flusher is elongate tubular or disc, is distributed with the aperture of diameter 0.2-2mm on the body of flusher or the card.
3. the production technique of preparation fatty acyl group according to claim 1-N methyl taurine natrium surfactant is characterized in that, described fat acyl chloride is for being selected from cocounut oil acyl chlorides, lauroyl chloride, cardamom acyl chlorides, palmityl chloride, stearyl chloride, oleoyl chloride, C
8-24At least a in the fat acyl chloride.
4. the production technique of preparation fatty acyl group according to claim 1-N methyl taurine natrium surfactant is characterized in that, the quality percentage composition of N methyl taurine sodium is 10%-60% in the described N methyl taurine sodium water solution; Temperature of reaction should be controlled below 40 ℃; The cooling of reactive system is by the external refrigeration equipment control of reactor.
5. according to the production technique of claim 1 or 4 described preparation fatty acyl group-N methyl taurine natrium surfactants, it is characterized in that the quality percentage composition of N methyl taurine sodium is 15%-40% in the described N methyl taurine sodium water solution; Temperature of reaction should be controlled below 30 ℃.
6. the production technique of preparation fatty acyl group according to claim 1-N methyl taurine natrium surfactant is characterized in that, described catalyzer and acid binding agent are for selecting NaOH, KOH, NaCO for use
3, KCO
3In at least a aqueous solution that is made into.
7. according to the production technique of claim 1 or 6 described preparation fatty acyl group-N methyl taurine natrium surfactants, it is characterized in that the pH value control of condensation reaction is below 10.
8. the production technique of preparation fatty acyl group according to claim 1-N methyl taurine natrium surfactant, it is characterized in that, after fat acyl chloride and acid-binding agent are added dropwise to complete, thick transferred product is to the emulsification pot, by the external heating installation heating of emulsification pot, the temperature of charge that raises gradually, to material liquefaction, bubble is eliminated; Temperature of charge control is below 80 ℃ in the emulsification pot.
9. the production technique of preparation fatty acyl group according to claim 1-N methyl taurine natrium surfactant is characterized in that, pH adjusts agent and selects organic acid for use or select mineral acid for use.
10. according to the production technique of claim 1 or 9 described preparation fatty acyl group-N methyl taurine natrium surfactants, it is characterized in that pH adjusts agent and selects hydrochloric acid for use, adjust the pH value below 8.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105771790A (en) * | 2016-05-18 | 2016-07-20 | 烟台大学 | Preparation method of protein-based surfactant |
| CN106397280A (en) * | 2016-11-23 | 2017-02-15 | 张家港格瑞特化学有限公司 | Preparation method of sodium lauroylmethyl taurate |
| CN106478466A (en) * | 2016-11-23 | 2017-03-08 | 张家港格瑞特化学有限公司 | A kind of preparation method of amino acid surfactant |
| CN106588709A (en) * | 2016-11-23 | 2017-04-26 | 张家港格瑞特化学有限公司 | Preparation method for sodium fatty acyl methyl taurate |
| CN107312511A (en) * | 2016-04-27 | 2017-11-03 | 中石化石油工程技术服务有限公司 | A kind of drilling fluid surfactant, its preparation method and drilling fluid |
| CN110041233A (en) * | 2019-05-20 | 2019-07-23 | 湖南丽臣奥威实业有限公司 | N- fatty acyl group-N methyl taurine sodium preparation method |
| CN110981759A (en) * | 2019-12-10 | 2020-04-10 | 上海嘉亨日用化学品有限公司 | Preparation method of N-acyl-N-methyltaurate and application of N-acyl-N-methyltaurate in silicone oil-free shampoo |
| CN112920094A (en) * | 2021-01-29 | 2021-06-08 | 江苏奥洁生物科技有限公司 | Method for adjusting production load and improving yield of N-methyl sodium taurate |
| CN113024401A (en) * | 2021-02-07 | 2021-06-25 | 广州花语精细化工有限公司 | Preparation process of amino acid surfactant capable of reducing byproducts |
| CN113444014A (en) * | 2021-06-28 | 2021-09-28 | 江苏金桥油脂科技有限公司 | System and method for continuously producing N-acyl amino acid surfactant |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107312511A (en) * | 2016-04-27 | 2017-11-03 | 中石化石油工程技术服务有限公司 | A kind of drilling fluid surfactant, its preparation method and drilling fluid |
| CN105771790A (en) * | 2016-05-18 | 2016-07-20 | 烟台大学 | Preparation method of protein-based surfactant |
| CN106397280A (en) * | 2016-11-23 | 2017-02-15 | 张家港格瑞特化学有限公司 | Preparation method of sodium lauroylmethyl taurate |
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| CN106588709A (en) * | 2016-11-23 | 2017-04-26 | 张家港格瑞特化学有限公司 | Preparation method for sodium fatty acyl methyl taurate |
| CN110041233A (en) * | 2019-05-20 | 2019-07-23 | 湖南丽臣奥威实业有限公司 | N- fatty acyl group-N methyl taurine sodium preparation method |
| CN110041233B (en) * | 2019-05-20 | 2021-09-10 | 湖南丽臣奥威实业有限公司 | Preparation method of N-fatty acyl-N-methyl sodium taurate |
| CN110981759A (en) * | 2019-12-10 | 2020-04-10 | 上海嘉亨日用化学品有限公司 | Preparation method of N-acyl-N-methyltaurate and application of N-acyl-N-methyltaurate in silicone oil-free shampoo |
| CN110981759B (en) * | 2019-12-10 | 2022-06-21 | 上海嘉亨日用化学品有限公司 | Preparation method of N-acyl-N-methyltaurate and application of N-acyl-N-methyltaurate in silicone oil-free shampoo |
| CN112920094A (en) * | 2021-01-29 | 2021-06-08 | 江苏奥洁生物科技有限公司 | Method for adjusting production load and improving yield of N-methyl sodium taurate |
| CN113024401A (en) * | 2021-02-07 | 2021-06-25 | 广州花语精细化工有限公司 | Preparation process of amino acid surfactant capable of reducing byproducts |
| CN113444014A (en) * | 2021-06-28 | 2021-09-28 | 江苏金桥油脂科技有限公司 | System and method for continuously producing N-acyl amino acid surfactant |
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Application publication date: 20130814 |