阅读说明：本技术 一种化工溶剂的制作方法 (Preparation method of chemical solvent ) 是由 郭徐良 万学明 张涛 于 2020-05-11 设计创作，主要内容包括：本发明公开了一种化工溶剂的制作方法,在加氢催化剂的作用下,苯甲酸在氢气作用下发生还原反应,反应结束后经过后处理得到所述的环己甲酸。本发明与现有技术相比优点在于：设计合理、反应收率高、成本更加低廉、具有更好的工业化应用意义。(The invention discloses a preparation method of a chemical solvent, wherein benzoic acid is subjected to a reduction reaction under the action of hydrogen under the action of a hydrogenation catalyst, and the cyclohexanecarboxylic acid is obtained through post-treatment after the reaction is finished. Compared with the prior art, the invention has the advantages that: reasonable design, high reaction yield, lower cost and better industrial application significance.)

1. A manufacturing method of a chemical solvent is characterized by comprising the following steps: under the action of a hydrogenation catalyst, benzoic acid is subjected to a reduction reaction under the action of hydrogen, and the cyclohexanecarboxylic acid is obtained through post-treatment after the reaction is finished.

2. The method for preparing chemical solvent according to claim 1, wherein the method comprises the following steps: the hydrogenation catalyst is obtained by treating nickel-aluminum-iron-copper alloy with an alkali solution.

3. The method for preparing chemical solvent according to claim 1, wherein the method comprises the following steps: the alkali solution is sodium hydroxide aqueous solution.

4. The method for preparing chemical solvent according to claim 1, wherein the method comprises the following steps: the pressure of the hydrogen is 0.5MPa to 4.5 MPa.

5. The method for preparing chemical solvent according to claim 1, wherein the method comprises the following steps: the solvent of the reduction reaction is one of ethylene glycol monomethyl ether, methanol, ethanol, isopropanol and n-butanol.

6. The method for preparing chemical solvent according to claim 1, wherein the method comprises the following steps: the temperature of the reduction reaction is 10-150 ℃.

Technical Field

The invention relates to the technical field of chemical synthesis, in particular to a preparation method of a chemical solvent.

Background

Chemical engineering is a science for researching the common law of chemical product production processes, the relation between human beings and chemical industry is very close, some chemical products play an epoch-making important role in the history of human development, and the production and application of the chemical products even represent a certain history stage of human civilization.

At present, chemical solvents are frequently used in the chemical industry, wherein the cyclohexanecarboxylic acid is usually colorless flaky or columnar crystals, is monoclinic prismatic crystals when condensed and odorless, but has valerian odor when liquefied or in solution, is an important organic synthesis raw material and is mainly used for synthesizing an anti-pregnancy 392 medicament, a schistosome new medicament, namely praziquantel medicament and the like; it can also be used as vulcanized rubber compatibilizer, petroleum clarifier, pesticide, dye and other organic compounds. The cyclohexanecarboxylic acid prepared in the current market has low yield, more residues and residual liquid, insufficient reaction, waste of raw materials, increased preparation cost and no contribution to industrial production.

Disclosure of Invention

The invention aims to solve the technical problem of providing a preparation method of a chemical solvent, which has the advantages of reasonable design, high reaction yield, lower cost and better industrial application significance.

In order to solve the technical problems, the technical scheme provided by the invention is as follows: under the action of hydrogenation catalyst, benzoic acid is subjected to reduction reaction under the action of hydrogen, and after the reaction is finished, the cyclohexanecarboxylic acid is obtained through post-treatment.

As an improvement, the hydrogenation catalyst is obtained by treating nickel-aluminum-iron-copper alloy with an alkali solution.

As an improvement, the alkali solution is sodium hydroxide aqueous solution.

As an improvement, the pressure of the hydrogen is 0.5MPa to 4.5 MPa.

As an improvement, the solvent of the reduction reaction is one of ethylene glycol monomethyl ether, methanol, ethanol, isopropanol and n-butanol.

As an improvement, the temperature of the reduction reaction is 10-150 ℃.

After adopting the structure, the invention has the following advantages: in the invention, a certain amount of iron and copper are added into the existing Ni-Al catalyst, so that the catalytic activity of the catalyst is effectively improved, the catalyst can be used for replacing a palladium catalyst for hydrogenation reduction of benzoic acid, the reduction reaction has high efficiency, the hydrogen pressure is too low, the reaction is not easy to fully carry out, the pressure is too high, the requirement on equipment is higher, preferably, the pressure of the hydrogen is 0.5-0.8 MPa, a reaction solvent can greatly influence the reaction result, most preferably, the solvent for the reduction reaction is ethanol, at the moment, the conversion rate is higher, the side reaction is less, the yield of the product is higher, and by adopting the nickel-aluminum-iron-copper catalyst, the cost of hydrogenation reduction of benzoic acid into cyclohexyl formic acid is effectively reduced, and the reaction efficiency is ensured, has a wide industrial application prospect.

Detailed Description

Structural formula (xvi):

the reaction mechanism is as follows:

the invention is implemented by pumping a proportional amount of liquid cyclohexanecarboxylic acid into a high-level metering tank from a transit tank (preheating feeding, discharging, overflow pipelines and the metering tank in advance, about 40 ℃), stopping pumping after the overflow outlet on the metering tank discharges liquid, starting a vacuum pump of a dissolving kettle to keep a micro negative pressure state, adding the proportional amount of benzoic acid from an inlet hole, sealing the inlet hole, stopping the vacuum pump, opening the vacuum pump, emptying, putting the cyclohexanecarboxylic acid in the metering tank into the kettle, turning and starting stirring after normal inching, heating up, preserving heat and dissolving, putting a proportional amount of catalyst into a filter in advance, reversely pumping the dissolved liquid into the hydrogenating kettle through a filter outlet, feeding the material, introducing nitrogen to replace air in the hydrogenating kettle, starting stirring, controlling the temperature of the kettle to be 80 +/-2 ℃ to guide hydrogen, keeping the kettle pressure to be 3.0-3.5 MPa for reaction for about 20 hours until no hydrogen is absorbed, sampling, taking the benzoic acid residue to be less than or equal to 0.2% as a reaction end point, after sampling is qualified, cooling to 35-40 ℃, discharging residual hydrogen in the kettle through a pressure relief buffer tank and an alkali liquor washing tank under the control of flow rate, discharging hydrogen to micro positive pressure (0.1MPa), and then introducing nitrogen for complete replacement; finally, the material is hydraulically transferred to a transfer pot, the catalyst is left in a filter and returns to a kettle together with the next batch of dissolved material for application, the filtrate is put into a negative pressure distillation tower, a first-stage vacuum pump is started to remove trace water (mainly containing water in the catalyst), then a second-stage vacuum pump and a third-stage vacuum pump are started for distillation, the product cyclohexanecarboxylic acid is obtained, the yield is 99.8 percent, no residual liquid or residue exists, trace cyclohexanecarboxylic acid odor in the operation processes of feeding, dissolving, distilling and the like is discharged, all emptying of the reaction kettle, the vacuum pump and the like are closed-loop introduced into an activated carbon fiber adsorption tower, the catalyst can be continuously applied for nearly 200 times, and after partial inactivation, the catalyst is returned to a supplier for reactivation, supplement and reuse.

The invention and its embodiments have been described above, without this being limitative. In summary, those skilled in the art should, without departing from the spirit of the present invention, devise similar structural modes and embodiments without inventively designing them, and shall fall within the scope of the present invention.