阅读说明：本技术 一种三氯蔗糖生产氯化步骤中低温连续配料的方法 (Method for low-temperature continuous batching in chlorination step of sucralose production ) 是由 张正颂 张�浩 付绪飞 沈孝峰 于 2020-05-23 设计创作，主要内容包括：本发明涉及一种三氯蔗糖氯代低温反应连续配料的方法,包括：把冷却至-1~5摄氏度的三氯乙烷与氯化亚砜,按一定流量比打入一级Y型管式反应器两个进口端进行混合,从一级Y型管式反应器出口端流出的混合液在冷凝器中急冷到0~5℃后进入混合液缓冲槽；b：将混合液和酯化定容液按一定的流量比,同时打入二级Y型管式反应器两个进口端进行混合,从二级Y型管式反应器出口端流出的二次混合液进行急冷到0~5℃后,打入搪瓷搅拌反应釜并冷却,二次混合液计量后送至高温反应釜进行高温。本发明过程工艺简单,可以实现低温反应的连续性,采用全自动化控制,减少了操作工的劳动强度,缩短了反应时间,降低能耗,大大提高了反应收率及生产效率。(The invention relates to a method for continuous proportioning of sucralose by low-temperature chlorination reaction, which comprises the following steps: trichloroethane and thionyl chloride cooled to the temperature of-1-5 ℃ are pumped into two inlet ends of a primary Y-shaped tubular reactor according to a certain flow ratio to be mixed, and mixed liquid flowing out of the outlet end of the primary Y-shaped tubular reactor is quenched in a condenser to the temperature of 0-5 ℃ and then enters a mixed liquid buffer tank; b: and simultaneously pumping the mixed liquid and the esterification constant volume liquid into two inlet ends of a secondary Y-shaped tubular reactor according to a certain flow ratio for mixing, quenching the secondary mixed liquid flowing out of the outlet end of the secondary Y-shaped tubular reactor to 0-5 ℃, pumping the secondary mixed liquid into an enamel stirring reaction kettle for cooling, metering the secondary mixed liquid, and delivering the secondary mixed liquid to the high-temperature reaction kettle for high temperature. The method has simple process, can realize the continuity of low-temperature reaction, adopts full-automatic control, reduces the labor intensity of operators, shortens the reaction time, reduces the energy consumption, and greatly improves the reaction yield and the production efficiency.)

1. A method for low-temperature continuous burdening in the chlorination step of sucralose production is characterized by comprising the following steps:

a: and (2) pumping the trichloroethane and the thionyl chloride cooled to the temperature of-1-5 ℃ into two inlet ends of a primary Y-shaped tubular reactor at the same time according to a certain flow ratio for mixing, wherein the molar ratio of the trichloroethane to the thionyl chloride is controlled to be 3.2-4.2: 1, rapidly cooling a mixed solution flowing out of the outlet end of a primary Y-shaped tubular reactor to 0-5 ℃ in a condenser, and then feeding the mixed solution into a mixed solution buffer tank;

b: the mixed liquid and the esterification constant volume liquid are pumped into two inlet ends of a second-stage Y-shaped tubular reactor to be mixed according to a certain flow ratio, the secondary mixed liquid flowing out of the outlet end of the second-stage Y-shaped tubular reactor is subjected to quenching in a condenser to 0-5 ℃, and then is pumped into an enamel stirring reaction kettle and is cooled, a circulating pump is circulated and stirred for 1 hour, finally, the secondary mixed liquid with uniform ingredients is continuously extracted from the outlet of the circulating pump, and the secondary mixed liquid is conveyed to the high-temperature reaction kettle to be subjected to high-temperature reaction after being metered.

2. The method of claim 1, wherein the esterification constant volume solution is DMF constant solution of sucrose-6-acetate, and the concentration of the esterification constant solution is one of the following: 280g/L, 290g/L, 300g/L, 310g/L, 320g/L, 330g/L, 340g/L, 350g/L and 360 g/L.

3. The method of claim 1, wherein in step b, the molar ratio of sucrose-6-acetate in the esterification solution to thionyl chloride in the mixed solution is controlled to be 1: 9.

The technical field is as follows:

the invention belongs to the technical field of sucralose production in the technical field of chemical industry, and particularly relates to a method for continuously blending materials in a chlorination workshop section at a low temperature in sucralose production.

Background art:

sucralose (Sucralose or TGS CNS: 19.016; INS: 955), also known as Sucralose, saccharan or 4, 1,6, -trichloro-4, 1,6, -trideoxy-semimilk sucrose, the english name: Sucralose. Sucralose is prepared by chlorination of sucrose as a raw material. The sucralose is a fresh sweetener, the sweetness is 800 times of that of the sucrose, the sweetness is pure and similar to that of the sucrose, the sucralose is not absorbed by human bodies, the biological accumulation is avoided, the safety is high, the application range is wide, and the sucralose can be used as a food additive to achieve the effects of reducing blood sugar and reducing sugar, so the sucralose industry develops rapidly in recent years. The production enterprises are gradually increased, and the yield is continuously improved.

The production capacity of the sucralose of an enterprise is continuously improved, the labor intensity is also continuously improved, in the chlorination step of the existing process production, the raw materials of trichloroethane and thionyl chloride are respectively metered and then are put into a reaction kettle, the chilled saline is used for pre-cooling to the required temperature, the temperature of the thionyl chloride is controlled to be 5-15 ℃, the temperature of the dropwise esterification constant volume liquid is controlled to be 5-15 ℃, and the mixture is put into a high-temperature kettle for high-temperature chlorination reaction after being uniformly stirred for 1 hour. This step is carried out in the middle of reation kettle absolutely, and reaction temperature is low, and reaction time is longer 6h, and the operation is intermittent type formula operation moreover, and the operation is frequent, and intensity of labour is big, and reaction condition is difficult to control, and artificially causes the technological index undulant frequently, and production efficiency is low, adopts manual site operation control moreover mostly, and artificial influence is great, and this reaction has restricted sucralose trade continuous industrial production greatly, is unfavorable for the amplification and the stability of sucralose production.

The invention content is as follows:

the invention aims to overcome the defects of the prior art and provide a method for continuously preparing materials at low temperature in sucralose production, which is simple to operate, high in efficiency, low in energy consumption and low in cost.

In order to achieve the above purpose, the process steps of the invention are as follows:

a method for low-temperature continuous burdening in the chlorination step of sucralose production is characterized by comprising the following steps:

a method for low-temperature continuous burdening in the chlorination step of sucralose production is characterized by comprising the following steps:

a: and (2) pumping the trichloroethane and the thionyl chloride cooled to the temperature of-1-5 ℃ into two inlet ends of a primary Y-shaped tubular reactor at the same time according to a certain flow ratio for mixing, wherein the molar ratio of the trichloroethane to the thionyl chloride is controlled to be 3.2-4.2: 1, rapidly cooling a mixed solution flowing out of the outlet end of a primary Y-shaped tubular reactor to 0-5 ℃ in a condenser, and then feeding the mixed solution into a mixed solution buffer tank;

b: the mixed liquid and the esterification constant volume liquid are pumped into two inlet ends of a second-stage Y-shaped tubular reactor to be mixed according to a certain flow ratio, the secondary mixed liquid flowing out of the outlet end of the second-stage Y-shaped tubular reactor is subjected to quenching in a condenser to 0-5 ℃, and then is pumped into an enamel stirring reaction kettle and is cooled, a circulating pump is circulated and stirred for 1 hour, finally, the secondary mixed liquid with uniform ingredients is continuously extracted from the outlet of the circulating pump, and the secondary mixed liquid is conveyed to the high-temperature reaction kettle to be subjected to high-temperature reaction after being metered.

The further technical scheme is as follows:

the esterification constant volume solution is DMF constant solution of sucrose-6-acetate, and the concentration of the esterification constant solution is one of the following: 280g/L, 290g/L, 300g/L, 310g/L, 320g/L, 330g/L, 340g/L, 350g/L and 360 g/L.

Controlling the molar ratio of sucrose-6-acetate in the esterification solution to thionyl chloride in the mixed solution to be 1: 9.

in the technical scheme, the Y-shaped tubular reactor is formed by manufacturing a stainless steel tube into a communicated Y shape, wherein the Y-shaped tubular reactor is provided with two inlet ends and one outlet end, so that two solutions can be continuously mixed, and the mixing efficiency of the two solutions is greatly improved.

Compared with the prior art, the technical scheme has the advantages that the primary and secondary Y-shaped tubular reactors are utilized to enable low-temperature batching to be continuous, intermittent batching in the prior art is avoided, continuous production operation is achieved, the scheme adopts dcs full-automatic control, production process indexes are controlled stably, fluctuation is small, the productivity level is greatly improved, the operation intensity of operators is greatly reduced, the operation environment is substantially improved, the effect of reducing energy consumption is achieved to a certain extent, the application prospect is very high, and feasibility is guaranteed for ten-thousand-ton large-scale industrial production.

Drawings

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

Detailed Description

To explain technical contents, structural characteristics, and objects and effects of the technical solutions in detail, the following detailed description is given with reference to the accompanying drawings in conjunction with the embodiments.