CN102921348A

CN102921348A - Synthetic process of novel SP-80 emulsifier

Info

Publication number: CN102921348A
Application number: CN2011102254367A
Authority: CN
Inventors: 刘勇; 徐文智; 黄文苏; 葛茜云
Original assignee: GUIZHOU JUENENG CHEMICAL CO Ltd
Current assignee: GUIZHOU JUENENG CHEMICAL CO Ltd
Priority date: 2011-08-08
Filing date: 2011-08-08
Publication date: 2013-02-13

Abstract

The invention provides a synthetic process of a novel SP-80 emulsifier; the purpose of the invention is to produce a high-quality emulsifier product, to provide a reasonable, simple, practical design process which can reduce production cost; a two-time catalytic reaction is performed to reduce the reaction temperature and to shorten the reaction time, so as to allow the reaction end to be easy to reach, to make the reaction complete, and to obtain higher yield. The method is to synthesize dehydrated sorbitan monooleate by a two-step method of first etherification and then esterification by using sorbitol and oleic acid as raw materials, and the method comprises the following steps: firstly performing the etherification reaction for 2-2.5 hours with a temperature requirement of 100-180 DEG C; adding a caustic soda catalyst (a primary catalyst of 4.8 Kg) at 90 DEG C, uniformly stirring, then performing the esterification reaction with a temperature requirement of 205-210 DEG C, when the esterification reaction is performed for 2.5 hours, adding the caustic soda catalyst (5.8 Kg) for the second time, reacting for 1 hour, pumping redundant free acids in vacuum, after the esterification reaction, cooling, precipitating, and filtering to obtain the finished product of SP-80.

Description

New type of S P-80 emulsifying agent synthesis technique

Technical field:

The present invention relates to a kind of New type of S P-80 emulsifying agent synthesis technique, belong to chemical field.

Background technology:

Along with carrying out in a deep going way of " development of the West Regions ", the further enforcement of " transferring electricity from the west to the east " engineering, in conjunction with the guidance spirit of " 12 planning ", Guizhou Province will do a good job of it with the traffic infrastructure construction of attaching most importance to, and Guizhou Province is turned into southwest land communications hinge.The quick-fried product of the people is " energy of energy industry, the basis of basic industries ", and it and capital construction are closely bound up, flourish along with capital construction, and the commercial explosive demand just is being the trend that increases substantially year by year.According to statistics, whole nation commercial explosive volume of production and marketing annual average rate of increase is about 7%, so the development potentiality in explosive market is very large, explosive adds auxiliary material, and to add agent be that explosive production must raw material, the explosive volume of production and marketing increases substantially, and will cause the growth of explosive auxiliary material additive demand.The quick-fried office of the national people adjusts whole civil explosive industry in recent years, has eliminated the ammonium nitrate-fuel oil powder type explosive, improves the consumption of latex explosive, and emulsifying agent SP-80 is as a kind of auxiliary material (addition is 1.5～2.5%) of latex explosive, and its consumption also increases considerably.Guizhou is huge chemical industry Co., Ltd to join subordinate subsidiary of group as Guizhou for a long time, for group company's explosive production line provides auxiliary material, with extend industrial chain and realization group company integration operation.Company has invested in 2004 and has produced 300 tons of emulsifying agent SP-80 production projects per year, but along with the requirement of the growth of product quantity in recent years and product quality is more and more higher, company has carried out capacity expansion revamping and research of technique in 2011 years, product quality is significantly improved with cost descend.

Modern crafts have been carried out many improvement to SP-80 synthetic.For example 1978, Hungary delivered one piece of article, had changed traditional one-step synthesis process with alkali as a catalyst, had adopted sorbierite elder generation dehydration etherificate, and then the two step method of carrying out esterification after the first etherificate of esterification with oleic acid.The U.S. delivered one piece of patent (USP 4,297,290) in 1981, had taked the similar way with Hungary, and its reaction also is to carry out in two steps, but the catalyst that adopts is different.Domestic since the end of the eighties, synthesis technique has adopted the two step method of esterification after the first etherificate.The technique of elder generation's etherificate, rear esterification is to make sorbierite be dehydrated into acid anhydride in the presence of acidic catalyst and decolorizer, carries out esterification with oleic acid again under base catalyst, and keeps higher vacuum in whole course of reaction.This method reaction condition makes moderate progress than one-step method, and impurity phase is to less, and color is more shallow; But still can not produce some specific (special) requirements high-viscosity products, and output capacity is low, and accessory substance is many, and can not satisfy the requirement of some special type latex explosive production.

Summary of the invention:

The object of the invention is to produce a kind of high-quality emulsifier production, propose a kind of reasonable, simple, easy, the design technology that can reduce production costs.

Technical scheme of the present invention is: with the sorbierite suction reaction kettle of the esterification of vacuum with ormal weight, add the phosphorous acid catalyst, heating makes sorbierite dehydration etherificate, and etherification reaction requires temperature to reach 100-180 degree centigrade, time 2-2.5 hour.With the oleic acid suction still preheater of vacuum with ormal weight, add caustic soda catalyst (for the first time catalyst 4.8Kg), stir, oleic acid is preheating to uniform temperature for subsequent use, sorbierite dehydration etherificate reaches requirement, with vacuum with in the oleic acid suction reaction kettle of the esterification, mixing of materials; Fast the temperature of esterified still temperature behind the batch mixing is raised to 190 ℃, namely begins esterification reaction, evenly with temperature from 190.℃ being raised to 205～215 ℃ carries out esterification, when esterification proceeds to 2.5h, adds base catalyst (5.8Kg) for the second time, react again 1h, take unnecessary free acid away with vacuum, esterification reaction is namely complete, and cooling, precipitation, filtration obtain finished product SP-80.

The invention has the beneficial effects as follows: easy to operate, realized the operability to emulsifier production in the technical process, carried out the quadric catalysis reaction and can reduce reaction temperature and Reaction time shorten, made reaction easily reach terminal point, make reaction carry out obtaining higher productive rate fully.

Description of drawings:

Accompanying drawing 1 is process chart of the present invention.

Accompanying drawing 2 is formulation content tables of the present invention.

Concrete embodiment:

A kind of New type of S P-80 emulsifying agent synthesis technique, its method step is: take sorbierite and oleic acid as raw material, adopt the two step synthesis sorbitan monooleate of esterification after the first etherificate, at first, etherification reaction requires temperature to reach 100-180 degree centigrade, time 2-2.5 hour.In the time of 90 degrees centigrade, add caustic soda catalyst (for the first time catalyst 4.8Kg), stir, then carry out esterification reaction, its reaction condition requires temperature to reach 205～210 degrees centigrade, when esterification proceeds to 2.5h, adds base catalyst (5.8Kg) for the second time, react again 1h, take unnecessary free acid away with vacuum, esterification reaction is namely complete, and cooling, precipitation, filtration obtain finished product SP-80.

The improvement principle of new synthesis process: esterification is a reversible reaction, along with the prolongation in reaction time and the rising of reaction temperature, esterification degree of depositing is better, but long reaction time and too high temperature make the easy coking of product, and accessory substance, impurity are many, the outward appearance poor fluidity, carry out the quadric catalysis reaction and can reduce reaction temperature and Reaction time shorten, make reaction easily reach terminal point, make reaction carry out obtaining higher productive rate fully.

Claims

1. New type of S P-80 emulsifying agent synthesis technique, its method step is: with the sorbierite suction reaction kettle of the esterification of vacuum with ormal weight, add the phosphorous acid catalyst, heating makes sorbierite dehydration etherificate; With the oleic acid suction still preheater of vacuum with ormal weight, add the caustic soda catalyst, a catalyst 4.8Kg stirs, and oleic acid is preheating to uniform temperature for subsequent use, sorbierite dehydration etherificate reaches requirement, with vacuum with in the oleic acid suction reaction kettle of the esterification, mixing of materials; Fast the temperature of esterified still temperature behind the batch mixing is raised to 190 ℃, namely begin esterification reaction, evenly temperature is raised to 205～215 ℃ from 190 ℃ and carries out esterification, when esterification proceeds to 2.5h, for the second time add base catalyst 5.8Kg, react again 1h, take unnecessary free acid away with vacuum, esterification reaction is namely complete, and cooling, precipitation, filtration obtain finished product SP-80.

2. according to the described a kind of New type of S P-80 emulsifying agent synthesis technique of claims, it is characterized in that sorbierite etherification reaction requirement temperature reaches 100-180 ℃, etherificate time 2-2.5h.

3. according to the described a kind of New type of S P-80 emulsifying agent synthesis technique of claims, it is characterized in that esterification requires temperature to reach 205-215 ℃, for the first time esterification time 2.5h, for the second time esterification time 1h.

4. according to the described a kind of New type of S P-80 emulsifying agent synthesis technique of claims, it is characterized in that on the basis of two step synthetic methods, proposed the technical concept of quadric catalysis reaction, namely in esterification reaction process, carry out the quadric catalysis reaction.