阅读说明：本技术 用四聚丙烯和氢氰酸合成n,n-二甲基癸胺的方法 (Method for synthesizing N, N-dimethyl decylamine by tetrapropylene and hydrocyanic acid ) 是由 张善荣 于 2021-01-26 设计创作，主要内容包括：本发明公开了一种用四聚丙烯和氢氰酸合成N,N-二甲基癸胺的方法,涉及石油化工产品的综合开发延伸利用技术领域,采用四聚丙烯和丙烯腈副产氢氰酸作为起始原料,在反应釜内加入四聚丙烯和溶剂,降温搅拌状态下滴加氢氰酸和催化剂,滴加结束保温反应,保温反应结束再加入甲醇和纯水搅拌反应,搅拌反应结束后经过中和、静置分相、蒸馏提纯等制得N,N-二甲基癸胺。本发明研发了一种新的N,N-二甲基癸胺的合成工艺,开发了四聚丙烯和丙烯腈副产氢氰酸新的高附加值的利用途径,使同为丙烯下游产品的四聚丙烯和丙烯腈副产氢氰酸产业链向精细化工产品延伸,提升丙烯下游产业链产品的经济效益。(The invention discloses a method for synthesizing N, N-dimethyldecylamine by tetrapropylene and hydrocyanic acid, which relates to the technical field of comprehensive development and extended utilization of petrochemical products. The invention develops a new synthesis process of N, N-dimethyldecylamine, develops a new high-added-value utilization way of tetrapropylene and acrylonitrile byproduct hydrocyanic acid, extends the tetrapropylene and acrylonitrile byproduct hydrocyanic acid industrial chain which is a downstream product of propylene to a fine chemical product, and improves the economic benefit of the downstream product of propylene.)

1. A method for synthesizing N, N-dimethyl decylamine by tetrapropylene and hydrocyanic acid is characterized in that: the method adopts tetrapropylene and acrylonitrile byproduct hydrocyanic acid as starting raw materials and comprises the following steps:

(1) the proportioning is as follows: tetrapropylene, solvent =1: 0.08-0.12;

adding tetrapropylene with the proportion of ingredients into the reaction kettle, adding the solvent with the proportion of ingredients into the reaction kettle under the stirring state,

mixing, and cooling to below 10 deg.C;

(2) the proportion of the ingredients is as follows: the tetrapropylene of step (1) is hydrocyanic acid catalyst =1: 0.13E

0.18: 0.5-0.9 adding hydrocyanic acid and a catalyst into the reaction kettle;

under the stirring state, dripping hydrocyanic acid and catalyst into the reaction kettle simultaneously, and controlling reaction in the dripping process

Keeping the temperature in the kettle to be not more than 30 ℃, keeping the temperature of 30-35 ℃ after dropwise adding, and reacting for 2 hours;

(3) the proportion of the ingredients is as follows: the tetrapropylene in the step (1) is methanol-water =1: 0.25-0.35: 0.4E

0.65 adding methanol and water into the reaction kettle;

after the heat preservation reaction in the step (2) is finished, adding methanol and water in a proportioning ratio into the reaction kettle,

mixing and stirring, and reacting for 2 hours;

(4) and (3) neutralization reaction:

transferring the material mixed and stirred in the step (3) and reacted into a neutralization kettle, and adding an alkaline regulator into the neutralization kettle

And the pH value of the material is 6-7;

(5) standing and separating:

transferring the material obtained after the neutralization reaction in the step (4) into a settling kettle for standing and layering, wherein the lower layer contains sulfur

Sending the acid salt water layer to a concentration kettle, separating water from salt-containing wastewater, and transferring the supernatant to a semi-finished product storage tank to obtain a semi-finished product;

(6) and (3) distillation and purification:

transferring the semi-finished product prepared in the step (5) into a distillation tower from a semi-finished product storage tank for distillation and purification,

removing low-boiling-point substances to obtain the finished product of the N, N-dimethyl decylamine.

2. The method of claim 1, wherein the N, N-dimethyldecylamine is synthesized from tetrapropylene and hydrocyanic acid, and the method comprises the following steps: the solvent in the step (1) is water or 30-75% methanol or a mixed solution of water and anhydrous methanol.

3. The method of claim 1, wherein the N, N-dimethyldecylamine is synthesized from tetrapropylene and hydrocyanic acid, and the method comprises the following steps: the catalyst in the step (2) is 98% sulfuric acid or fuming sulfuric acid or mixed sulfuric acid of 98% sulfuric acid and fuming sulfuric acid.

4. The method of claim 1, wherein the N, N-dimethyldecylamine is synthesized from tetrapropylene and hydrocyanic acid, and the method comprises the following steps: and (3) the alkaline regulator in the step (4) is liquid alkali or potassium hydroxide or sodium carbonate or ammonia.

5. The method of claim 1, wherein the N, N-dimethyldecylamine is synthesized from tetrapropylene and hydrocyanic acid, and the method comprises the following steps: and (4) transferring the water separated from the concentration kettle in the step (5) to the step (3) for recycling.

Technical Field

The invention relates to the technical field of comprehensive development and extension utilization of petrochemical products, in particular to a method for synthesizing N, N-dimethyldecylamine by tetrapropylene and hydrocyanic acid.

Background

N, N-Dimethyldecylamine, also known as decaalkyldimethyl tertiary amine, dimethyl N-decylamine, colorless to pale yellow transparent liquid in appearance, molecular formula: C12H27N, molecular weight 185.35, flash point 91.6 ℃ and boiling point 234 ℃.

The N, N-dimethyl decylamine is mainly used for producing dialkyl quaternary ammonium salt, cationic surfactant or amphoteric amine oxide surfactant, is widely applied to the industries of daily chemical personal care, disinfectants, fabric washing, softening, anti-corrosion printing and dyeing auxiliaries, emulsifiers, detergents and foaming agents, and is also used for producing pesticides, dyes, medical intermediates and plastic additives.

Tetrapropylene (Propylene Tetramer), also known as N-dodecene, Propylene Tetramer, etc., colorless liquid, obtained by Propylene tetramerization, or separated from C10-C14 fraction obtained by paraffin cracking, can be used for producing straight chain or branched chain type alkylbenzene, making dodecylphenol polyoxyethylene ether, dodecylphenol, alkyl diphenyl ether sodium disulfonate, producing detergent, surfactant, plasticizer, petroleum additive, lubricant additive, synthesizing tetracosene, directly synthesizing tert-dodecyl mercaptan with hydrogen sulfide, producing T746 antirust agent with maleic anhydride, and has wide application, but no technical research and development information and report of tetrapropylene used for fine chemical product N, N-dimethyldecylamine are found.

Acrylonitrile is produced by the ammoxidation of propylene with by-products of acetonitrile, hydrocyanic acid and ammonium sulfate.

The acrylonitrile and the tetrapropylene are downstream products of propylene, which is a petrochemical product, and the industrial chain of the downstream products of propylene is prolonged by synthesizing N, N-dimethyldecylamine from the tetrapropylene and hydrocyanic acid, which is a byproduct of an acrylonitrile device.

At present, little information is provided about research and development experiments and development of synthesizing N, N-dimethyldecylamine by utilizing tetrapropylene and acrylonitrile byproduct hydrocyanic acid in China, and information related to industrial production of N, N-dimethyldecylamine is not common.

Disclosure of Invention

The invention aims to solve the technical problem of providing a method for synthesizing N, N-dimethyl decylamine by tetrapropylene and hydrocyanic acid.

In order to solve the technical problems, the invention provides the following technical scheme: a method for synthesizing N, N-dimethyl decylamine by tetrapropylene and hydrocyanic acid adopts the tetrapropylene and acrylonitrile byproduct hydrocyanic acid as starting raw materials, and comprises the following steps:

(1) the proportioning is as follows: tetrapropylene, solvent =1: 0.08-0.12;

adding tetrapropylene in a proportioning ratio into a reaction kettle, adding a solvent in the proportioning ratio under a stirring state, uniformly mixing, and cooling to below 10 ℃;

(2) the proportion of the ingredients is as follows: adding hydrocyanic acid and a catalyst into a reaction kettle, wherein the tetrapropylene is prepared from hydrocyanic acid and the catalyst is =1: 0.13-0.18: 0.5-0.9;

dropwise adding hydrocyanic acid and an acid catalyst into the reaction kettle simultaneously under the stirring state, controlling the temperature in the reaction kettle not to exceed 30 ℃ in the dropwise adding process, keeping the temperature at 30-35 ℃ after the dropwise adding is finished, and reacting for 2 hours;

(3) the proportion of the ingredients is as follows: adding methanol and water into a reaction kettle, wherein the tetrapropylene in the step (1) is methanol and water, and the ratio of the methanol to the water is =1: 0.25-0.35: 0.4-0.65;

after the heat preservation reaction in the step (2) is finished, adding methanol and water in a proportioning ratio into the reaction kettle, mixing and stirring, and reacting for 2 hours;

(4) and (3) neutralization reaction:

transferring the material mixed and stirred in the step (3) to a neutralization kettle, and neutralizing the pH value of the material by using an alkaline regulator to be 6-7;

(5) standing and separating:

transferring the material subjected to the neutralization reaction in the step (4) into a settling kettle for standing and layering, conveying the lower sulfate salt-containing water layer to a concentration kettle, separating water from salt-containing wastewater, and transferring the supernatant into a semi-finished product storage tank to obtain a semi-finished product;

(6) and (3) distillation and purification:

and (4) transferring the semi-finished product prepared in the step (5) into a distillation tower from a semi-finished product storage tank for distillation and purification, and removing low-boiling-point substances to obtain a finished product of the N, N-dimethyl decylamine.

Preferably, the solvent in the step (1) is water or 30-75% methanol or a mixed solution of water and anhydrous methanol.

Preferably, the catalyst in step (2) is 98% sulfuric acid or oleum or a mixed sulfuric acid of 98% sulfuric acid and oleum.

Preferably, the alkaline regulator in step (4) is liquid alkali or potassium hydroxide or sodium carbonate or ammonia.

Preferably, the water separated from the concentration kettle in the step (5) is transferred to the step (3) for recycling.

The invention adopts the structure and has the following advantages:

1. the invention develops a new synthesis process of N, N-dimethyl decylamine, and the aim of industrial production can be achieved through flow design;

2. the invention develops a new high-added-value utilization way of the tetrapropylene and acrylonitrile byproduct hydrocyanic acid, so that the tetrapropylene and acrylonitrile byproduct hydrocyanic acid industrial chain which is a downstream propylene product is extended to fine chemical products, and the economic benefit of the downstream propylene industrial chain product is improved;

3. the synthetic process flow route designed by the invention is simple and clear, and under the condition of no mature and referable technical data, equipment configuration related to the process flow can adopt a reaction kettle, a mechanical pump and a rectifying tower which are made of conventional materials and have conventional specifications according to physicochemical properties of various raw materials and intermediates, so that industrial mass production can be realized.

Drawings

FIG. 1 is a process flow diagram of the present invention.

Detailed Description

To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings.

Example 1

(1) Adding 150 kg of tetrapropylene into a reaction kettle, adding 12 kg of water under a stirring state to fully and uniformly mix the tetrapropylene and the water, and cooling the temperature in the reaction kettle to below 10 ℃;

(2) reducing the temperature of materials in the reaction kettle to 5-10 ℃, simultaneously dropwise adding 21 kg of hydrocyanic acid and 75 kg of 98% sulfuric acid catalyst into the reaction kettle, keeping the materials in the reaction kettle in a stirring state in the dropwise adding process of the hydrocyanic acid and the 98% sulfuric acid catalyst, controlling the reaction temperature not to exceed 30 ℃, keeping the temperature of the materials in the kettle within the range of 30-35 ℃ after the dropwise adding of the hydrocyanic acid and the 98% sulfuric acid catalyst is finished, and keeping the temperature of the materials in the kettle for 2 hours;

(3) after the reaction is carried out for 2 hours under the heat preservation condition, adding 37.5 kg of methanol and 60 kg of water into the reaction kettle again, fully stirring and mixing, and continuing the reaction for 2 hours;

(4) transferring the material mixed and reacted in the step (3) into a neutralization kettle, adding an alkaline regulator into the neutralization kettle by taking the pH value of the material in the kettle as a standard of 6-7, and carrying out neutralization reaction on the material for 2-4 hours;

(5) transferring the material after the neutralization reaction into a settling kettle for standing and layering, wherein the upper layer is an N, N-dimethyl N-decylamine semi-finished product, the lower layer is a sulfate salt water-containing layer, the upper layer semi-finished product is transferred into a semi-finished product storage tank, and the lower layer is a sulfate salt water-containing layer which is transferred into a concentration kettle;

(6) transferring the N, N-dimethyl N-decylamine semi-finished product in the semi-finished product storage tank into a distillation tower for distillation and purification, removing low-boiling-point substances, preparing 161.5 kg of N, N-dimethyl N-decylamine finished product, and calculating the reaction yield of 94.26%;

(7) and distilling and concentrating the salt-containing wastewater in the concentration kettle, and separating water and sulfate.

Example 2

(1) Adding 160 kg of tetrapropylene into a reaction kettle, adding 16 kg of 30% methanol solution under stirring to fully and uniformly mix the tetrapropylene and the 30% methanol solution, and cooling the temperature in the reaction kettle to below 10 ℃;

(2) reducing the temperature of materials in the reaction kettle to 5-10 ℃, simultaneously dropwise adding 26 kg of hydrocyanic acid and 110 kg of fuming sulfuric acid catalyst into the reaction kettle, keeping the materials in the reaction kettle in a stirring state in the dropwise adding process of the hydrocyanic acid and the fuming sulfuric acid catalyst, controlling the reaction temperature not to exceed 30 ℃, keeping the temperature of the materials in the kettle within the range of 30-35 ℃ after the dropwise adding of the hydrocyanic acid and the fuming sulfuric acid catalyst is finished, and carrying out heat preservation reaction on the materials for 2 hours;

(3) after the reaction is carried out for 2 hours under the heat preservation condition, adding 55 kg of methanol and 80 kg of water into the reaction kettle again, fully stirring and mixing, and continuing the reaction for 2 hours;

(4) transferring the material mixed and reacted in the step (3) into a neutralization kettle, adding an alkaline regulator into the neutralization kettle by taking the pH value of the material in the kettle as a standard of 6-7, and carrying out neutralization reaction on the material for 2-4 hours;

(5) transferring the material after the neutralization reaction into a settling kettle for standing and layering, wherein the upper layer is an N, N-dimethyl N-decylamine semi-finished product, the lower layer is a sulfate salt water-containing layer, the upper layer semi-finished product is transferred into a semi-finished product storage tank, and the lower layer is a sulfate salt water-containing layer which is transferred into a concentration kettle;

(6) transferring the N, N-dimethyl N-decylamine semi-finished product in the semi-finished product storage tank into a distillation tower for distillation and purification, removing low-boiling-point substances to obtain 173 kg of N, N-dimethyl N-decylamine finished product, and calculating the reaction yield to be 94.66%;

(7) and distilling and concentrating the salt-containing wastewater in the concentration kettle, and separating water and sulfate.

Example 3

(1) Adding 170 kg of tetrapropylene into a reaction kettle, adding 20 kg of 50% methanol solution under stirring to fully and uniformly mix the tetrapropylene and the 50% methanol solution, and cooling the temperature in the reaction kettle to below 10 ℃;

(2) reducing the temperature of materials in the reaction kettle to 5-10 ℃, simultaneously dropwise adding 30 kg of hydrocyanic acid and 135 kg of 98% sulfuric acid and fuming sulfuric acid of an acidic mixed catalyst in a ratio of 1:1 into the reaction kettle, keeping the materials in the reaction kettle in a stirring state in the dropwise adding process of the hydrocyanic acid and the acidic mixed catalyst, controlling the reaction temperature to be not more than 30 ℃, keeping the temperature of the materials in the kettle within a range of 30-35 ℃ after the dropwise adding of the hydrocyanic acid and the acidic mixed catalyst is finished, and carrying out heat preservation reaction on the materials for 2 hours;

(3) after the reaction is carried out for 2 hours under the heat preservation condition, adding 65 kg of methanol and 100 kg of water into the reaction kettle again, fully stirring and mixing, and continuing the reaction for 2 hours;

(4) transferring the material mixed and reacted in the step (3) into a neutralization kettle, adding an alkaline regulator into the neutralization kettle by taking the pH value of the material in the kettle as a standard of 6-7, and carrying out neutralization reaction on the material for 2-4 hours;

(5) transferring the material after the neutralization reaction into a settling kettle for standing and layering, wherein the upper layer is an N, N-dimethyl N-decylamine semi-finished product, the lower layer is a sulfate salt water-containing layer, the upper layer semi-finished product is transferred into a semi-finished product storage tank, and the lower layer is a sulfate salt water-containing layer which is transferred into a concentration kettle;

(6) transferring the N, N-dimethyl N-decylamine semi-finished product in the semi-finished product storage tank into a distillation tower for distillation and purification, removing low-boiling-point substances to obtain 183.5 kg of N, N-dimethyl N-decylamine finished product, and calculating the reaction yield to be 95.02%;

(7) and distilling and concentrating the salt-containing wastewater in the concentration kettle, and separating water and sulfate.

Example 4

(1) Adding 150 kg of tetrapropylene into a reaction kettle, adding 20 kg of water under a stirring state to fully and uniformly mix the tetrapropylene and the water, and cooling the temperature in the reaction kettle to below 10 ℃;

(2) reducing the temperature of materials in the reaction kettle to 5-10 ℃, simultaneously dropwise adding 26 kg of hydrocyanic acid and 135 kg of catalyst of 98% sulfuric acid catalyst into the reaction kettle, keeping the materials in the reaction kettle in a stirring state in the dropwise adding process of the hydrocyanic acid and the 98% sulfuric acid catalyst, controlling the reaction temperature not to exceed 30 ℃, keeping the temperature of the materials in the kettle within the range of 30-35 ℃ after the dropwise adding of the hydrocyanic acid and the 98% sulfuric acid catalyst is finished, and keeping the temperature of the materials in the kettle for 2 hours;

(3) after the reaction is carried out for 2 hours under the condition of heat preservation, adding 55 kg of methanol and 100 kg of water into the reaction kettle again, fully stirring and mixing, and continuing the reaction for 2 hours;

(4) transferring the material mixed and reacted in the step (3) into a neutralization kettle, adding an alkaline regulator into the neutralization kettle by taking the pH value of the material in the kettle as a standard of 6-7, and carrying out neutralization reaction on the material for 2-4 hours;

(5) transferring the material after the neutralization reaction into a settling kettle for standing and layering, wherein the upper layer is an N, N-dimethyl N-decylamine semi-finished product, the lower layer is a sulfate salt water-containing layer, the upper layer semi-finished product is transferred into a semi-finished product storage tank, and the lower layer is a sulfate salt water-containing layer which is transferred into a concentration kettle;

(6) transferring the N, N-dimethyl N-decylamine semi-finished product in the semi-finished product storage tank into a distillation tower for distillation and purification, removing low-boiling-point substances to obtain 163.1 kg of N, N-dimethyl N-decylamine finished product, and calculating the reaction yield to be 95.20%;

(7) and distilling and concentrating the salt-containing wastewater in the concentration kettle, and separating water and sulfate.

Example 5

(1) Adding 160 kg of tetrapropylene into a reaction kettle, adding 16 kg of 30% methanol solution under stirring to fully and uniformly mix the tetrapropylene and the 30% methanol solution, and cooling the temperature in the reaction kettle to below 10 ℃;

(2) reducing the temperature of materials in the reaction kettle to 5-10 ℃, simultaneously dropwise adding 30 kg of hydrocyanic acid and 110 kg of fuming sulfuric acid catalyst into the reaction kettle, keeping the materials in the reaction kettle in a stirring state in the dropwise adding process of the hydrocyanic acid and the fuming sulfuric acid catalyst, controlling the reaction temperature not to exceed 30 ℃, keeping the temperature of the materials in the kettle within the range of 30-35 ℃ after the dropwise adding of the hydrocyanic acid and the fuming sulfuric acid catalyst is finished, and carrying out heat preservation reaction on the materials for 2 hours;

(3) after the reaction is carried out for 2 hours under the heat preservation condition, adding 65 kg of methanol and 80 kg of water into the reaction kettle again, fully stirring and mixing, and continuing the reaction for 2 hours;

(4) transferring the material mixed and reacted in the step (3) into a neutralization kettle, adding an alkaline regulator into the neutralization kettle by taking the pH value of the material in the kettle as a standard of 6-7, and carrying out neutralization reaction on the material for 2-4 hours;

(5) transferring the material after the neutralization reaction into a settling kettle for standing and layering, wherein the upper layer is an N, N-dimethyl N-decylamine semi-finished product, the lower layer is a sulfate salt water-containing layer, the upper layer semi-finished product is transferred into a semi-finished product storage tank, and the lower layer is a sulfate salt water-containing layer which is transferred into a concentration kettle;

(6) transferring the N, N-dimethyl N-decylamine semi-finished product in the semi-finished product storage tank into a distillation tower for distillation and purification, removing low-boiling-point substances to obtain 174.6 kg of N, N-dimethyl N-decylamine finished product, and calculating the reaction yield to be 95.54%;

(7) and distilling and concentrating the salt-containing wastewater in the concentration kettle, and separating water and sulfate.

Example 6

(1) Adding 170 kg of tetrapropylene into a reaction kettle, adding 12 kg of 50% methanol solution under stirring to fully and uniformly mix the tetrapropylene and the 50% methanol solution, and cooling the temperature in the reaction kettle to below 10 ℃;

(2) reducing the temperature of materials in the reaction kettle to 5-10 ℃, simultaneously dropwise adding 26 kg of hydrocyanic acid and 75 kg of 98% sulfuric acid and fuming sulfuric acid of an acidic mixed catalyst in a ratio of 1:1 into the reaction kettle, keeping the materials in the reaction kettle in a stirring state in the dropwise adding process of the hydrocyanic acid and the acidic mixed catalyst, controlling the reaction temperature to be not more than 30 ℃, keeping the temperature of the materials in the kettle within a range of 30-35 ℃ after the dropwise adding of the hydrocyanic acid and the acidic mixed catalyst is finished, and carrying out heat preservation reaction on the materials for 2 hours;

(3) after the reaction is carried out for 2 hours under the heat preservation condition, adding 37.5 kg of methanol and 60 kg of water into the reaction kettle again, fully stirring and mixing, and continuing the reaction for 2 hours;

(4) transferring the material mixed and reacted in the step (3) into a neutralization kettle, adding an alkaline regulator into the neutralization kettle by taking the pH value of the material in the kettle as a standard of 6-7, and carrying out neutralization reaction on the material for 2-4 hours;

(5) transferring the material after the neutralization reaction into a settling kettle for standing and layering, wherein the upper layer is an N, N-dimethyl N-decylamine semi-finished product, the lower layer is a sulfate salt water-containing layer, the upper layer semi-finished product is transferred into a semi-finished product storage tank, and the lower layer is a sulfate salt water-containing layer which is transferred into a concentration kettle;

(6) transferring the N, N-dimethyl N-decylamine semi-finished product in the semi-finished product storage tank into a distillation tower for distillation and purification, removing low-boiling-point substances to obtain 185.6 kg of N, N-dimethyl N-decylamine finished product, and calculating the reaction yield of 95.61%;

(7) and distilling and concentrating the salt-containing wastewater in the concentration kettle, and separating water and sulfate.

Example 7

(1) Adding 150 kg of tetrapropylene into a reaction kettle, adding 16 kg of water under a stirring state to fully and uniformly mix the tetrapropylene and the water, and cooling the temperature in the reaction kettle to below 10 ℃;

(2) reducing the temperature of materials in the reaction kettle to 5-10 ℃, simultaneously dropwise adding 21 kg of hydrocyanic acid and 135 kg of 98% sulfuric acid catalyst into the reaction kettle, keeping the materials in the reaction kettle in a stirring state in the dropwise adding process of the hydrocyanic acid and the 98% sulfuric acid catalyst, controlling the reaction temperature not to exceed 30 ℃, keeping the temperature of the materials in the kettle within the range of 30-35 ℃ after the dropwise adding of the hydrocyanic acid and the 98% sulfuric acid catalyst is finished, and keeping the temperature of the materials in the kettle for 2 hours;

(3) after the reaction is carried out for 2 hours under the condition of heat preservation, adding 55 kg of methanol and 100 kg of water into the reaction kettle again, fully stirring and mixing, and continuing the reaction for 2 hours;

(4) transferring the material mixed and reacted in the step (3) into a neutralization kettle, adding an alkaline regulator into the neutralization kettle by taking the pH value of the material in the kettle as a standard of 6-7, and carrying out neutralization reaction on the material for 2-4 hours;

(5) transferring the material after the neutralization reaction into a settling kettle for standing and layering, wherein the upper layer is an N, N-dimethyl N-decylamine semi-finished product, the lower layer is a sulfate salt water-containing layer, the upper layer semi-finished product is transferred into a semi-finished product storage tank, and the lower layer is a sulfate salt water-containing layer which is transferred into a concentration kettle;

(6) transferring the N, N-dimethyl N-decylamine semi-finished product in the semi-finished product storage tank into a distillation tower for distillation and purification, removing low-boiling-point substances to obtain 162.3 kg of N, N-dimethyl N-decylamine finished product, and calculating the reaction yield to be 94.72%;

(8) and distilling and concentrating the salt-containing wastewater in the concentration kettle, and separating water and sulfate.

Example 8

(1) Adding 160 kg of tetrapropylene into a reaction kettle, adding 20 kg of 30% methanol solution under stirring to fully and uniformly mix the tetrapropylene and solvent water, and cooling the temperature in the reaction kettle to below 10 ℃;

(2) reducing the temperature of materials in the reaction kettle to 5-10 ℃, simultaneously dropwise adding 30 kg of hydrocyanic acid and 75 kg of fuming sulfuric acid catalyst into the reaction kettle, keeping the materials in the reaction kettle in a stirring state in the dropwise adding process of the hydrocyanic acid and the fuming sulfuric acid catalyst, controlling the reaction temperature not to exceed 30 ℃, keeping the temperature of the materials in the kettle within the range of 30-35 ℃ after the dropwise adding of the hydrocyanic acid and the fuming sulfuric acid catalyst is finished, and keeping the temperature of the materials in the kettle for 2 hours;

(3) after the reaction is carried out for 2 hours under the heat preservation condition, adding 37.5 kg of methanol and 80 kg of water into the reaction kettle again, fully stirring and mixing, and continuing the reaction for 2 hours;

(4) transferring the material mixed and reacted in the step (3) into a neutralization kettle, adding an alkaline regulator into the neutralization kettle by taking the pH value of the material in the kettle as a standard of 6-7, and carrying out neutralization reaction on the material for 2-4 hours;

(5) transferring the material after the neutralization reaction into a settling kettle for standing and layering, wherein the upper layer is an N, N-dimethyl N-decylamine semi-finished product, the lower layer is a sulfate salt water-containing layer, the upper layer semi-finished product is transferred into a semi-finished product storage tank, and the lower layer is a sulfate salt water-containing layer which is transferred into a concentration kettle;

(6) transferring the N, N-dimethyl N-decylamine semi-finished product in the semi-finished product storage tank into a distillation tower for distillation and purification, removing low-boiling-point substances, and obtaining 171.2 kg of N, N-dimethyl N-decylamine finished product with the calculated reaction yield of 94.20%;

(7) and distilling and concentrating the salt-containing wastewater in the concentration kettle, and separating water and sulfate.

Example 9

(1) Adding 170 kg of tetrapropylene into a reaction kettle, adding 16 kg of 50% methanol solution under stirring to fully and uniformly mix the tetrapropylene and the 50% methanol solution, and cooling the temperature in the reaction kettle to below 10 ℃;

(2) reducing the temperature of materials in the reaction kettle to 5-10 ℃, simultaneously dropwise adding 21 kg of hydrocyanic acid and 110 kg of 98% sulfuric acid and fuming sulfuric acid of an acidic mixed catalyst in a ratio of 1:1 into the reaction kettle, keeping the materials in the reaction kettle in a stirring state in the dropwise adding process of the hydrocyanic acid and the acidic mixed catalyst, controlling the reaction temperature to be not more than 30 ℃, keeping the temperature of the materials in the kettle within a range of 30-35 ℃ after the dropwise adding of the hydrocyanic acid and the acidic mixed catalyst is finished, and carrying out heat preservation reaction on the materials for 2 hours;

(3) after the reaction is carried out for 2 hours under the heat preservation condition, adding 65 kg of methanol and 60 kg of water into the reaction kettle again, fully stirring and mixing, and continuing the reaction for 2 hours;

(4) transferring the material mixed and reacted in the step (3) into a neutralization kettle, adding an alkaline regulator into the neutralization kettle by taking the pH value of the material in the kettle as a standard of 6-7, and carrying out neutralization reaction on the material for 2-4 hours;

(5) transferring the material after the neutralization reaction into a settling kettle for standing and layering, wherein the upper layer is an N, N-dimethyl N-decylamine semi-finished product, the lower layer is a sulfate salt water-containing layer, the upper layer semi-finished product is transferred into a semi-finished product storage tank, and the lower layer is a sulfate salt water-containing layer which is transferred into a concentration kettle;

(6) transferring the N, N-dimethyl N-decylamine semi-finished product in the semi-finished product storage tank into a distillation tower for distillation and purification, removing low-boiling-point substances, preparing 182.2 kg of N, N-dimethyl N-decylamine finished product, and calculating the reaction yield of 93.87%;

(7) and distilling and concentrating the salt-containing wastewater in the concentration kettle, and separating water and sulfate.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.