CN203128459U - Preparation system of tertiary amine - Google Patents
Preparation system of tertiary amine Download PDFInfo
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- CN203128459U CN203128459U CN 201220708814 CN201220708814U CN203128459U CN 203128459 U CN203128459 U CN 203128459U CN 201220708814 CN201220708814 CN 201220708814 CN 201220708814 U CN201220708814 U CN 201220708814U CN 203128459 U CN203128459 U CN 203128459U
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Abstract
The utility model relates to a preparation system of tertiary amine. The preparation system comprises a dimethylamine carburetor, an amination reaction kettle, an amination fractionating tower, a first-stage condenser, a second-stage condenser, a third-stage condenser and an amination fan buffer tank, and is characterized in that the third-stage condenser is connected with a newly-arranged circulating gas water washing tower, and the circulating gas water washing tower performs self-circulation through a circulating pump of the circulating gas water washing tower. The preparation system has the beneficial effects that the circulating gas water washing tower is newly arranged in the preparation system of the tertiary amine, the property that monomethyl amine, dimethyl amine and trimethyl amine are easily soluble in water is utilized for introducing mixed gas of hydrogen, trimethyl amine, a small amount of monomethyl amine and a small amount of dimethyl amine in a reactor into the circulating gas water washing tower, after the monomethyl amine, the dimethyl amine and the trimethyl amine are absorbed by water, the pure hydrogen is obtained, then the pure hydrogen is introduced into the amination reaction kettle in a circulating manner, and then the hydrogen consumption of the whole reaction processes is zero.
Description
Technical field
The utility model belongs to the detergent raw material preparation system, relates in particular to a kind of preparation system of tertiary amine.
Background technology
Along with broad masses of the people's standard of living improves rapidly, the consumption of domestic detergent progressively increases.According to statistics, Chinese detergent market sales volume on average with annual 12% speed increment, by year 4.5 kilograms of calculating of consumption per capita, reach the international average level of consumption, and the articles for washing total amount in China every year will reach more than 2,300 ten thousand tons.China is washing powder output the first in the world at present, and products such as washing composition, shampoo have become popular consumer goods and requisite.Detergent applications has become the important industry field of concerning the people's livelihood.
Fat tertiary amine is a kind of common detergent raw material, is used for hair soft agent, hair conditioner, liquid lotion suds booster.Alcohol one-step technology be one of tertiary amine production most important method, principal reaction be Fatty Alcohol(C12-C14 and C12-C18) and dimethylamine under the effect of catalyzer, dewater the generation tertiary amine.Certainly, it is the primary condition that guarantees that amination reaction carries out smoothly that suitable temperature of reaction cooperates controlled hydrogen pressure.
The preparation system of tertiary amine comprises dimethylamine vaporizer, amination reaction still, amination separation column, first-stage condenser, secondary condenser, three grades of condensers and amination blower fan surge tank, described amination separation column is communicated with by pipeline with the amination reaction still, described amination separation column connects with the first-stage condenser that is connected successively and secondary condenser again respectively with the amination reaction still, described secondary condenser is connected with amination blower fan surge tank, and the amination separation column is connected with dimethylamine vaporizer and three grades of condensers respectively.In tertiary amine was produced, the product quality indicator of amination reaction Working Procedure Controlling had remaining alcohol, primary/secondary amine, working substance etc., and distillation process can effectively be regulated and control color and luster, working substance content etc.Above-mentioned quality index has very big influence to the working substance content of quaternary ammonium salt, color and luster, physico-chemical parameter such as water-soluble.
The reaction of Fatty Alcohol(C12-C14 and C12-C18) and dimethylamine is undertaken by following formula:
In the presence of high reactivity and selectivity amination catalysis, the mixed gas of dimethylamine and hydrogen fed be heated in the liquid phase Fatty Alcohol(C12-C14 and C12-C18) of temperature of reaction, Fatty Alcohol(C12-C14 and C12-C18) namely with the dimethylamine reaction, slough an one's share of expenses for a joint undertaking water, generate alkyl dimethyl tertiary amide.Water generation reaction is vaporized and is taken away by hydrogen, thereby reaction is carried out fully.But when carrying out above-mentioned amination reaction, also some side reactions of association mainly contain:
Wherein, the reactant Monomethylamine is obtained by the dimethylamine disproportionation.And generate Trimethylamine 99 simultaneously in disproportionation reaction, and when reaching a certain amount of, the Trimethylamine 99 in the recycle gas can hinder the hydrogen effect of facing of dimethylamine in the main reaction, and speed of reaction and yield are reduced.In a word, side reaction not only will consume expensive Fatty Alcohol(C12-C14 and C12-C18) and dimethylamine more, also will increase the complicacy of separation, and influence the purity of product to a certain extent.
The utility model content
The purpose of this utility model is to overcome the deficiency of above-mentioned technology, a kind of preparation system of tertiary amine is provided, can in the presence of catalyzer, prepare tertiary amine by Fatty Alcohol(C12-C14 and C12-C18) and dimethylamine gas, by accelerating main reaction and suppress the carrying out of side reaction, thereby realize the purpose of high produced in yields high purity tertiary amine.
The utility model for achieving the above object, by the following technical solutions: a kind of preparation system of tertiary amine, comprise the dimethylamine vaporizer, the amination reaction still, the amination separation column, first-stage condenser, secondary condenser, three grades of condensers and amination blower fan surge tank, described amination separation column is communicated with by pipeline with the amination reaction still and carries out thermal exchange, described amination separation column connects the water that generates for separating of reaction with the first-stage condenser that is connected successively and secondary condenser again respectively with the amination reaction still, described secondary condenser is connected the gas circulation of finishing the amination system with amination blower fan surge tank, the amination separation column is connected with dimethylamine vaporizer and three grades of condensers respectively, it is characterized in that: described three grades of condensers are connected with the recycle gas water scrubber that increases newly, and described recycle gas water scrubber is undertaken one by the recycle gas water scrubber recycle pump, two, the self-circulation that Trimethylamine 99 absorbs.
Described amination blower fan surge tank feeds recycle gas in the connected recycle gas water scrubber by the amination roots blower.
Beneficial effect: newly-increased recycle gas water scrubber in the preparation system of tertiary amine, when the reaction conversion ratio of described main reaction proceeds to 80%-90%, hydrogen in the reactor, Trimethylamine 99, a small amount of Monomethylamine, a small amount of dimethylamine mixed gas are fed recycle gas water scrubber, with one, two, after the Trimethylamine 99 water absorbs, obtain pure hydrogen recirculation and feed in the amination reaction still, making the hydrogen consumption of entire reaction flow process is zero.The optimization technology of preparation tertiary amine can make hydrogen gas consumption low, has reduced the Trimethylamine 99 environmentally safe, saves the reaction times, and Trimethylamine 99 can be used as by-product sale.One ton of tertiary amine of every production can reduce consumption 5～10 mark cubic meters of hydrogen after the use present technique, and the amination reaction time shortens 2～2.5 hours (single batch), and one ton of tertiary amine of every production can reclaim 15～20Kg Trimethylamine 99.
Description of drawings
Fig. 1 is the flow sheet of optimizing back preparation tertiary amine;
Fig. 2 is the flow sheet of former preparation tertiary amine.
Among the figure: 1, dimethylamine vaporizer, 2, the amination reaction still, 3, amination separation column 4, first-stage condenser 5, secondary condenser, 6, three grades of condensers, 7, amination blower fan surge tank, 8, the amination roots blower, 9, recycle gas water scrubber 10, recycle gas water scrubber recycle pump.
Embodiment
Describe embodiment of the present utility model in detail below in conjunction with preferred embodiment.
Embodiment
A kind of preparation system of tertiary amine, comprise dimethylamine vaporizer 1, amination reaction still 2, amination separation column 3, first-stage condenser 4, secondary condenser 5, three grades of condensers 6, amination blower fan surge tank 7, amination roots blower 8, recycle gas water scrubber 9, recycle gas water scrubber recycle pump 10, described amination separation column is communicated with by pipeline with the amination reaction still, described amination separation column connects with the first-stage condenser that is connected successively and secondary condenser again respectively with the amination reaction still, described secondary condenser is connected with amination blower fan surge tank, the amination separation column is connected with dimethylamine vaporizer and three grades of condensers respectively, described three grades of condensers are connected with the recycle gas water scrubber 9 that increases newly, and described recycle gas water scrubber is undertaken one by recycle gas water scrubber recycle pump 10, two, the self-circulation that Trimethylamine 99 absorbs.Described amination blower fan surge tank feeds hydrogen in the connected recycle gas water scrubber by amination roots blower 8.
Production stage is as follows:
Amination reaction still 2 is carried out nitrogen replacement earlier go out air in the still, carry out hydrogen exchange again and go out the interior nitrogen of still, after the interior oxygen of analysis still is qualified, use nitrogen is pressed into 5～5.5 tons Fatty Alcohol(C12-C14 and C12-C18) (12,12/14 Fatty Alcohol(C12-C14 and C12-C18) or 18/16 Fatty Alcohol(C12-C14 and C12-C18)) in the amination reaction still, hydrogen partial will the emptying along with being pressed into of material, with behind the heat-conducting oil heating amination reaction still to 170 in the chuck ℃, begin to stir, and with hydrogen make keep in the still certain pressure (0.05～0.15MPa), with reducing catalyst under the hydrogen effect 45 minutes; Open the steam valve of dimethylamine vaporizer, amination reaction still material temperature rise to 190 ℃ is treated in preheating 10 minutes, and beginning slowly feeds dimethylamine; The control temperature of reaction feeds the dimethylamine of 800kg in 210～220 ℃, when the primary alconol transformation efficiency reaches 80%--90%, the Trimethylamine 99 gas that reaction generates is drawn reactant systems; Utilize in the amination reaction still in the gaseous component partial pressure value of hydrogen to determine that gas phase is drawn the amination reaction still carries out the time that water absorbs, when the dividing potential drop of hydrogen is lower than 40%--60%, amination reaction still gas phase is drawn wash processing; In the reaction initial stage, speed of response is very fast, but the carrying out along with reaction, because the inert component that the Trimethylamine 99 that disproportionation reaction generates reacts for this reason, its continuous accumulation in gas phase has reduced the dividing potential drop of hydrogen and dimethylamine, simultaneously since Trimethylamine 99 in the chemisorbed on catalyst effect, reduced hydrogen and the dimethylamine adsorptive capacity on catalyzer, at the catalytic efficiency that reduces catalyzer simultaneously, also increased the possibility that generates other side reactions, therefore when the primary alconol transformation efficiency reaches 80%--90%, the Trimethylamine 99 gas that reaction generates is drawn the reaction system, can accelerate the carrying out of subsequent reactions greatly, reduced the possibility that side reaction takes place simultaneously, improved the yield of main reaction, Trimethylamine 99 can be used as by-product sale in addition; Reaction end confirms according to the internal control quality index that through middle control analysis reaction finishes the back material and enters down road sedimentation operation.In amination reaction, a small amount of Monomethylamine that the dimethylamine disproportionation reaction produces and Trimethylamine 99 be Monomethylamine and the two alkyl tertiary amines of Fatty Alcohol(C12-C14 and C12-C18) reaction generation wherein.And Trimethylamine 99 can't react with Fatty Alcohol(C12-C14 and C12-C18), becomes the part and the dimethylamine that contain amine tail gas and enters in the recycle gas water scrubber.
The reactor gas phase absorbs the processing wastewater that produces through water can obtain the Trimethylamine 99 byproduct through rectifying, and the gas that absorption process produces is pure hydrogen after drying, feeds in the amination still through recycle compressor.
Amination reaction is squeezed into down operation with material and is carried out sedimentation after finishing.After sedimentation for some time, the catalyzer of sedimentation is returned the amination still apply mechanically, supernatant liquid changes still kettle over to and distills.With clear liquid suction distillation tower in the sedimentation still, under vacuum condition, a spot of dimethylamine that remains in the material also enters the absorption tower absorption.Because of different tertiary amine boiling point differences, the control Heating temperature namely gets product after the finished product alkyl tertiary amine steamed, and distillation still residue be two alkyl tertiary amines, and it is temporary to enter the height groove that boils, unified processing.The interference effect of Trimethylamine 99 is reduced in the reactor, and the reaction times shortens.
The above only is preferred embodiment of the present utility model, is not structure of the present utility model is done any pro forma restriction.Every foundation technical spirit of the present utility model all still belongs in the scope of the technical solution of the utility model any simple modification, equivalent variations and modification that above embodiment does.
Claims (2)
1. the preparation system of a tertiary amine, comprise the dimethylamine vaporizer, the amination reaction still, the amination separation column, first-stage condenser, secondary condenser, three grades of condensers and amination blower fan surge tank, described amination separation column is communicated with by pipeline with the amination reaction still and carries out thermal exchange, described amination separation column connects the water that generates for separating of reaction with the first-stage condenser that is connected successively and secondary condenser again respectively with the amination reaction still, described secondary condenser is connected the gas circulation of finishing the amination system with amination blower fan surge tank, the amination separation column is connected with dimethylamine vaporizer and three grades of condensers respectively, it is characterized in that: described three grades of condensers are connected with the recycle gas water scrubber that increases newly, and described recycle gas water scrubber is undertaken one by the recycle gas water scrubber recycle pump, two, the self-circulation that Trimethylamine 99 absorbs.
2. the preparation system of tertiary amine according to claim 1, it is characterized in that: described amination blower fan surge tank feeds recycle gas in the connected recycle gas water scrubber by the amination roots blower.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201220708814 CN203128459U (en) | 2012-12-18 | 2012-12-18 | Preparation system of tertiary amine |
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| CN 201220708814 CN203128459U (en) | 2012-12-18 | 2012-12-18 | Preparation system of tertiary amine |
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| CN203128459U true CN203128459U (en) | 2013-08-14 |
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| CN 201220708814 Expired - Fee Related CN203128459U (en) | 2012-12-18 | 2012-12-18 | Preparation system of tertiary amine |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112619588A (en) * | 2020-12-02 | 2021-04-09 | 辽宁圣德华星化工有限公司 | Tertiary amine production device and production method thereof |
| CN114105777A (en) * | 2021-12-10 | 2022-03-01 | 江苏万盛大伟化学有限公司 | Preparation method of low-residual alcohol monoalkyl fatty tertiary amine |
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2012
- 2012-12-18 CN CN 201220708814 patent/CN203128459U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112619588A (en) * | 2020-12-02 | 2021-04-09 | 辽宁圣德华星化工有限公司 | Tertiary amine production device and production method thereof |
| CN114105777A (en) * | 2021-12-10 | 2022-03-01 | 江苏万盛大伟化学有限公司 | Preparation method of low-residual alcohol monoalkyl fatty tertiary amine |
| CN114105777B (en) * | 2021-12-10 | 2024-03-12 | 江苏万盛大伟化学有限公司 | Preparation method of low-residual alcohol mono-alkyl fatty tertiary amine |
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Legal Events
| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130814 Termination date: 20181218 |
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| CF01 | Termination of patent right due to non-payment of annual fee |