阅读说明：本技术 一种氯苯甘油醚的干燥及加工方法 (Method for drying and processing chlorphenesin ) 是由 郑阿龙 沈寒晰 张金峰 郭鹏涛 习娟 刘彦婷 徐亚霞 于 2020-12-22 设计创作，主要内容包括：本发明公开了一种氯苯甘油醚的干燥及加工方法,其工艺步骤是将精制氯苯甘油醚产品加入真空搅拌釜中进行惰性气体置换保护,使搅拌釜真空度控制在0.06～0,098mpa,对搅拌釜内的进行蒸发加热,待物料有流动性后,开始搅拌,蒸发至物料恒重或者水分检测小于0.3％,得到干燥合格产品；对干燥合格产品可根据用户需求导向加工成粉状、片状、复配及颗粒型等多种所需产品。本发明提高了氯苯甘油醚产品干燥效率,操作环境安全,工艺时间缩短,可再次提纯从而使产品品质二次提升,产品含量达到99.5％以上,熔融态外观接近无色透亮,产品剂型多样可选,降低了生产成本,实现了提质增效的工艺理念,也为该工艺及产品的工业化应用创造了条件。(The invention discloses a method for drying and processing chlorphenesin, which comprises the following steps of adding a refined chlorphenesin product into a vacuum stirring kettle for inert gas replacement protection, controlling the vacuum degree of the stirring kettle to be 0.06-0,098 mpa, carrying out evaporation heating on the stirring kettle, starting stirring after the material has fluidity, evaporating until the material has constant weight or the moisture content is less than 0.3%, and obtaining a dried qualified product; the dried qualified product can be processed into various required products such as powder, sheet, compound, granule and the like according to the requirement of a user. The method improves the drying efficiency of the chlorphenesin product, has safe operation environment and shortened process time, can be purified again so as to improve the product quality for the second time, has the product content of more than 99.5 percent, has nearly colorless and transparent appearance in a molten state, has various and selectable product formulations, reduces the production cost, realizes the process concept of quality improvement and efficiency improvement, and also creates conditions for the industrial application of the process and the product.)

1. A method for drying and processing chlorphenesin is characterized by comprising the following process steps:

1.1 adding a chlorphenesin product with the moisture content of 15-50 percent after recrystallization by a water-alcohol mixed solvent into a solvent filled with N₂Or CO₂Inert gas replacement protection is carried out in a gas vacuum stirring kettle, the adding amount of the chlorphenesin product is 1/2-2/3 of the volume of the stirring kettle, a vacuum pump is utilized to control the vacuum degree of the stirring kettle at 0.06-0,098 mpa, evaporation heating is carried out in the stirring kettle,heating for 3-8 h at 80-120 ℃, stirring after the material has fluidity, and evaporating until the material has constant weight or the water content is less than 0.3%, thus obtaining qualified dry material;

1.2 maintaining the dried qualified material at 80-90 ℃, and performing vacuum heat filtration of clean hot air blowing on the material by using a precision filter with the precision below 5um to obtain molten material filtrate with the purity of more than 99.5%;

1.3 the filtered molten state material filtrate can be processed by four conditions, namely:

processing a powdery product, namely rapidly cooling the filtered molten material filtrate to 20-40 ℃ by cold water or air within 5-15 min, crushing the cooled and solidified material by a crusher or a ball mill, sieving with a 400-1000-mesh sieve, and packaging to obtain a powdery product of dry chlorphenesin; or

Processing a sheet product, namely rapidly cooling the filtered molten material filtrate to 20-40 ℃ by cold water or air within 5-15 min, slicing the cooled and solidified material by a slicing machine, wherein the sheet thickness is 1-3 mm, and packaging to obtain the dried chlorphenesin sheet product; or

Processing a compound product, namely adding benzyl alcohol or phenethyl alcohol into the filtered molten material filtrate for compounding, wherein the adding amount of the benzyl alcohol or the phenethyl alcohol is 1-5 times of the weight of the raw material chlorphenesin product, and obtaining the compound type anti-corrosive bactericide product of the dry chlorphenesin after compounding and packaging; or

And (3) processing a granular product, namely adding sodium sulfate or carboxymethyl cellulose which accounts for 1-5 per mill of the weight of the raw chlorphenesin product into the filtered molten material filtrate, uniformly mixing, kneading and granulating by using a granulator to obtain the granular product of the dry chlorphenesin after the granules are packaged, wherein the grain size is 1-2 mm.

Technical Field

The invention belongs to the technical field of preparation of daily chemical products, relates to a processing method of a mildew inhibitor chlorphenesin product, and particularly relates to a drying and processing method of a chlorphenesin product.

Background

Chlorophenol ether (chlorphenisin), also known as chlorophenol ether and chlorphenesin, is a mildew inhibitor with excellent performance. In the aspect of medicine, chlorphenesin serving as an antifungal medicine is suitable for resisting diseases such as fungi, bacteria, vaginal mold, trichomonad and the like; in the aspect of cosmetics, chlorphenesin can effectively resist gram-positive bacteria, gram-negative bacteria and the like, and the chlorphenesin hydrochloride can be widely applied to products such as nail polish, skin care agents, hair dyes and the like internationally in recent years.

At present, chlorphenesin refined by a conventional process (such as a water-alcohol mixed solvent recrystallization method) known in the art is generally a moisture-containing solid, the moisture content is 15-50%, and the moisture-containing solid has the problems of influencing the product quality, being unfavorable for the transportation and storage of the product, influencing the dissolution and use of the residual solvent and the like, so the chlorphenesin must be dried in the actual sale and use links of the product. The traditional drying method of wet solids in p-chlorphenesin mostly adopts a normal pressure or reduced pressure drying mode, equipment is selected from bipyramid rotary vacuum drying equipment, flash evaporation drying equipment, a double-blade dryer, fixed bed drying equipment and the like, different drying equipment is selected according to different refined materials, and the drying temperature can not be higher than the melting point of the materials according to the principle. The problems existing in the traditional mode are that the drying temperature is low (30-60 ℃), the drying time is long (generally 24 hours or even longer), the drying efficiency is low (the water content of the product is 40-60 ℃ at 30-60 ℃), the product is mainly a single powder product after drying, the dosage form is single, the adjustment is not easy, the product purity is not high, and the product cannot be purified again.

In recent years, some departments and enterprises at home and abroad adopt the processes of organic solvent crystallization and low-temperature drying to process and process chlorphenesin products, namely chlorphenesin is firstly dissolved in organic solvents such as methanol, chloroform and the like, then is quickly dried at low temperature, and then the dried materials are processed into slices or granules and the like. The organic solvent has the characteristics of low boiling point and high volatility, so that the chlorphenesin product is extremely easy to dry quickly, and the drying efficiency is high. However, the method has the defects that most of the used organic solvents are toxic, harmful, inflammable and explosive articles, the environment and the personal safety are harmed, and the potential safety hazard is great. There are also some departments dealing with the product by using a water-reconstituted refined solvent, but the drying of the product is relatively cumbersome and difficult. Because the melting point of the pure dry product is 77-79 ℃, the moisture content of the refined product is different, the melting point of the wet product is different, the higher the moisture content is, the lower the melting point of the wet product is, therefore, normal-pressure low-temperature drying or vacuum drying is generally adopted firstly, so that the water evaporation is slow, the drying time is long, the drying efficiency is low, and the product is easy to melt.

The above reflects the problems of single product dosage form, incapability of purification, long drying time, low efficiency, use of toxic and harmful solvents and the like existing in the drying and processing processes of chlorphenesin products at present, and the problems seriously restrict the continuous healthy development of related enterprises. Therefore, from the angle of process technology improvement, the method breaks through the current technical barrier, breaks through the constraint of the original drying process mode, adopts a high-efficiency and safe product drying processing technology, reduces energy consumption and material consumption, improves the drying efficiency and processing diversity of chlorphenesin, and has important positive significance for long-term development of enterprises.

Disclosure of Invention

The invention aims to solve the problems in the prior art and provides a method for drying and processing chlorphenesin products, which has the advantages of scientific and reasonable design route, safety, environmental protection, high drying efficiency, diversified products, convenient processing and good economic benefit.

The technical solutions adopted to achieve the above objects of the invention are as follows.

A method for drying and processing chlorphenesin comprises the following process steps:

1. adding a chlorphenesin product with the moisture content of 15-50% after recrystallization by using a water-alcohol mixed solvent into a solvent filled with N₂Or CO₂Carrying out inert gas replacement protection in a gas vacuum stirring kettle, wherein the adding amount of a chlorphenesin product is 1/2-2/3 of the volume of the stirring kettle, controlling the vacuum degree of the stirring kettle at 0.06-0,098 mpa by utilizing a vacuum pump, carrying out evaporation heating on the stirring kettle for 3-8 h at the heating temperature of 80-120 ℃, starting stirring after the material has fluidity, and evaporating until the material has constant weight or the moisture content is less than 0.3%, thus obtaining qualified drying;

2. maintaining the dried qualified material at 80-90 ℃, and performing vacuum heat filtration of clean hot air blowing on the material by using a precision filter with the precision below 5 mu m to obtain molten material filtrate with the purity of more than 99.5%;

3. the filtered molten material filtrate can be processed in four conditions, namely:

processing a powdery product, namely rapidly cooling the filtered molten material filtrate to 20-40 ℃ by cold water or air within 5-15 min, crushing the cooled and solidified material by a crusher or a ball mill, sieving with a 400-1000-mesh sieve, and packaging to obtain a powdery product of dry chlorphenesin; or

Processing a sheet product, namely rapidly cooling the filtered molten material filtrate to 20-40 ℃ by cold water or air within 5-15 min, slicing the cooled and solidified material by a slicing machine, wherein the sheet thickness is 1-3 mm, and packaging to obtain the dried chlorphenesin sheet product; or

Processing a compound product, namely adding benzyl alcohol or phenethyl alcohol into the filtered molten material filtrate for compounding, wherein the adding amount of the benzyl alcohol or the phenethyl alcohol is 1-5 times of the weight of the raw material chlorphenesin product, and obtaining the compound type anti-corrosive bactericide product of the dry chlorphenesin after compounding and packaging; or

And (3) processing a granular product, namely adding sodium sulfate or carboxymethyl cellulose which accounts for 1-5 per mill of the weight of the raw chlorphenesin product into the filtered molten material filtrate, uniformly mixing, kneading and granulating by using a granulator to obtain the granular product of the dry chlorphenesin after the granules are packaged, wherein the grain size is 1-2 mm.

In step 1 of the technical scheme of the invention, the used vacuum stirring kettle can adopt a stirring drying kettle (a glass three-neck flask), an enamel kettle or a stainless steel kettle and the like; the used vacuum pump can be selected from a water circulation vacuum pump, a Roots mechanical vacuum pump or other vacuum pumps meeting the vacuum requirement; the heating heat source can be hot water, water vapor or heat conducting oil, hot air, etc.

In the steps of the invention, as the technical scheme that the chlorphenesin product is added into the vacuum stirring kettle for inert gas replacement protection is adopted, the refined chlorphenesin can improve the drying temperature, strengthen the drying heat transfer effect and shorten the drying time; in the drying step, flammable, explosive, toxic and harmful organic solvents are abandoned, the melting point limitation is broken through according to the characteristics of low melting point, easiness in melting and stability in melting of the product, the original drying time can be shortened from 24 hours to 1-3 hours by means of smooth utilization, the drying efficiency is improved, and the dried material can be processed into various required products such as powder, sheets, compound products, granules and the like according to the requirement of a user. In addition, the product obtained by the conventional drying method is a solid phase and a single phase, the purity is not high enough, and the product cannot be purified again, but the product is a liquid phase by adopting the method of the invention, wherein the melting point is high or insoluble impurities are just filtered and removed, the product purity is improved again, and the product purity can reach more than 99.5 percent.

The process is suitable for drying and processing wet products with low melting point, stable product molten state and high decomposition temperature, and is particularly suitable for processing wet products containing the water chlorphenesin.

Drawings

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

Detailed Description

Example 1

230g of a refined product of chlorphenesin with the moisture content of 50 percent after recrystallization by a water-alcohol mixed solvent is taken, added into a 500ml three-neck flask, subjected to nitrogen replacement protection, heated at the temperature of 80-85 ℃, the vacuum degree of 0.090Mpa and the heating time of 50min until the product is constant in weight, kept at the temperature of 80-90 ℃, subjected to heat filtration by a precision 3um filter, purged by clean hot air at the temperature of 80-90 ℃ to obtain a molten product, rapidly cooled by cold water at the temperature of 25 ℃, cooled for 10min, solidified, crushed by a crusher, sieved by a 600-mesh sieve, weighed and packaged. Sampling detection shows that the water content is 0.2%, the content reaches 99.68%, the molten state is colorless transparent liquid, the product content is not less than 99.5%, and the molten state of the product is close to the technological index requirement of the colorless transparent liquid.

Example 2

300kg of refined chlorphenesin product with the moisture content of 45 percent after recrystallization by using a water-alcohol mixed solvent is added into a 500l vacuum kettle for nitrogen replacement protection, the heating temperature is 90-100 ℃, the vacuum degree is 0.093Mpa, the heating time is 43min, the product constant weight is kept at 80-90 ℃, the temperature is kept at 80-90 ℃, the product is subjected to heat filtration by a precision 3-micron filter and is swept by clean hot air at 80-90 ℃ to obtain a molten state product, the molten state product is rapidly cooled by cold water at 25 ℃ for 10min, the temperature is reduced for 10min, the product is solidified, and the product is cut into 1.5 mm slices by a slicing machine, weighed and packaged. Sampling detection shows that the water content is 0.12%, the content reaches 99.78%, the molten state is colorless transparent liquid, the product content is not less than 99.5%, and the molten state of the product is close to the technological index requirement of the colorless transparent liquid.

Example 3

Taking 280kg of refined chlorphenesin product recrystallized by a water-alcohol mixed solvent, wherein the moisture content is 43%, adding the refined chlorphenesin product into a 500l vacuum kettle for nitrogen replacement protection, heating to 90-100 ℃, the vacuum degree is 0.093Mpa, the heating time is 50min, the product has constant weight, keeping the temperature at 80-90 ℃, performing heat filtration by a precision 3um filter, purging by clean hot air at 80-90 ℃ to obtain a molten product, adding 1kg of carboxymethyl cellulose, stirring and mixing uniformly, kneading and granulating by a granulator to obtain the particle size of about 2 mm, weighing, and packaging. And (3) sampling and detecting a molten product, wherein the water content is 0.09%, the content reaches 99.81%, the molten state is colorless transparent liquid, the content of the product is not less than 99.5%, and the molten state of the product is close to the technological index requirement of the colorless transparent liquid.

Example 4

350kg of refined chlorphenesin product recrystallized by using a water-alcohol mixed solvent and having a moisture content of 50 percent are added into a 500l vacuum kettle, nitrogen replacement protection is performed, the heating temperature is 90-100 ℃, the vacuum degree is 0.093Mpa, the heating time is 55min, the product is constant in weight, the temperature is kept at 80-90 ℃, the product is subjected to heat filtration by a precision 3-micron filter, clean hot air blowing is performed at 80-90 ℃ to obtain a molten product, then 400 kg of functional auxiliary agent benzyl alcohol is added under stirring for dissolving and compounding, the product is weighed after being dissolved uniformly, and the product is packaged. And (3) sampling and detecting a molten product, wherein the water content is 0.089 percent, the content reaches 99.78 percent, the molten product is colorless transparent liquid, the content of the product is not less than 99.5 percent, and the molten state of the product is close to the technological index requirement of the colorless transparent liquid.