CN113620796A - Continuous preparation method and system of dibenzoyl methane - Google Patents

Continuous preparation method and system of dibenzoyl methane Download PDF

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Publication number
CN113620796A
CN113620796A CN202110707833.1A CN202110707833A CN113620796A CN 113620796 A CN113620796 A CN 113620796A CN 202110707833 A CN202110707833 A CN 202110707833A CN 113620796 A CN113620796 A CN 113620796A
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heating zone
rectifying tower
esterification reaction
feeding pipe
condensation
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CN113620796B (en
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李兑
童庆军
李平
张国靓
王艳
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ANHUI JIAXIAN FUNCTIONAL AUXILIARY CO LTD
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ANHUI JIAXIAN FUNCTIONAL AUXILIARY CO LTD
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/45—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by condensation
    • C07C45/455—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by condensation with carboxylic acids or their derivatives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/245—Stationary reactors without moving elements inside placed in series
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/0215—Sulfur-containing compounds
    • B01J31/0225—Sulfur-containing compounds comprising sulfonic acid groups or the corresponding salts
    • B01J35/19—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
    • B01J2231/40—Substitution reactions at carbon centres, e.g. C-C or C-X, i.e. carbon-hetero atom, cross-coupling, C-H activation or ring-opening reactions
    • B01J2231/49—Esterification or transesterification
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/584—Recycling of catalysts

Abstract

The invention discloses a continuous preparation method and a system of dibenzoyl methane, wherein the preparation method comprises the following steps: taking benzoic acid and methanol as raw materials, carrying out esterification reaction for 3-6h at the temperature of 100-110 ℃ under the catalytic action of a composite catalyst, and rectifying after the reaction is finished to obtain methyl benzoate; directly mixing methyl benzoate with a xylene solution containing acetophenone and sodium methoxide, carrying out claisen condensation reaction, and after the reaction is finished, crystallizing and filtering to obtain dibenzoyl methane; the invention overcomes the defects of the prior art, ensures continuous production, improves the reaction speed, shortens the reaction time and improves the yield of the dibenzoyl methane.

Description

Continuous preparation method and system of dibenzoyl methane
Technical Field
The invention relates to the technical field of dibenzoyl methane production, and particularly belongs to a continuous preparation method and system of dibenzoyl methane.
Background
China is a large country for PVC production, processing and consumption, the market growth speed of the environment-friendly PVC heat stabilizer dibenzoyl methane is kept at 10% or more, and the market growth speed of the environment-friendly PVC heat stabilizer dibenzoyl methane is increased along with the health of environmental regulations and the concern on product quality safety, at present, lead salt stabilizers are mainly used in domestic markets, but the use of lead salt heat stabilizers is greatly limited in the future along with the implementation of new environmental protection laws in China and the gradual enhancement of environmental protection consciousness of people. Meanwhile, with the revision of national environmental protection laws and the continuous enhancement of environmental protection awareness of people, the lead-free heat stabilizer has huge market potential. In 2016, 12 months, Ministry of industry and communications, Ministry of scientific technology, Ministry of environmental protection and other departments of 'substitution of toxic and harmful raw materials (products) encouraged by China for catalogue 2016' encourages to replace lead salt heat stabilizers with heat stabilizers such as calcium-based and calcium-zinc.
The commonly used environment-friendly lead-free heat stabilizer mainly comprises calcium stearate, zinc stearate and the like. When the single stearate is used alone, the problems of 'zinc burn', initial color difference, insufficient weather resistance and the like occur, and a core material dibenzoyl methane and other heat stabilizer additives are required to be matched for use. However, dibenzoyl methane has key technical problems in industrial production, mainly including: (1) the industrial synthesis technology has low yield, large consumption of raw materials and high production cost; (2) the byproducts are more, and the subsequent treatment difficulty is high; (3) the industrial drying technology has low efficiency, limits the production capacity and cannot meet the increasing market demand; (4) the product has poor color and large smell, and influences the color and long-term stability of the PVC product; (5) the three-waste treatment technology is immature, and the normal production of the product is restricted.
Disclosure of Invention
The invention aims to provide a continuous preparation method and a continuous preparation system of dibenzoyl methane, which solve the problems of low yield, large raw material consumption and high production cost of the industrial synthesis technology of dibenzoyl methane.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a continuous preparation method of dibenzoyl methane comprises the following steps:
s1, taking benzoic acid and methanol as raw materials, carrying out esterification reaction for 3-6h at the temperature of 100-110 ℃ under the catalytic action of a composite catalyst, and rectifying after the reaction is finished to obtain methyl benzoate;
s2, directly mixing methyl benzoate with a xylene solution containing acetophenone and sodium methoxide, carrying out claisen condensation reaction, and after the reaction is finished, crystallizing and filtering to obtain dibenzoyl methane;
the composite catalyst is a mixture of p-toluenesulfonic acid and concentrated sulfuric acid, wherein the mass of the p-toluenesulfonic acid is 5-10% of that of the concentrated sulfuric acid, and the addition amount of the composite catalyst is 1-3% of the total mass of benzoic acid and methanol.
Preferably, the ratio of the amount of the substances of benzoic acid and methanol is 1: 4-7.
Preferably, the claisen condensation reaction is carried out at three gradient temperatures of 80-90 ℃, 130-.
A continuous dibenzoyl methane preparation system comprises an esterification reaction kettle, a rectifying tower, a temporary storage tank and a condensation tank, an upper feeding pipe and a lower feeding pipe are arranged on the side wall of the esterification reaction kettle, the lower feeding pipe is arranged below the liquid level in the esterification reaction kettle, the bottom of the rectifying tower is connected with the bottom of the esterification reaction kettle through two material conveying pipes, the lower part of the rectifying tower is provided with a liquid separating plate which divides the bottom of the rectifying tower into a left part and a right part, the feed delivery pipes at the bottom of the rectifying tower are respectively positioned at the two sides of the liquid separation plate, the top of the rectifying tower is connected with the condensation tank through a pipeline, the temporary storage tank is arranged on a pipeline between the rectifying tower and the condensation tank, the pipeline between the temporary storage tank and the condensation tank is also connected with a feed pipe, and the feeding pumps are respectively arranged on the upper feeding pipe, the lower feeding pipe, the feeding pipe and the pipeline between the feeding pipe and the temporary storage tank.
Preferably, the condensation tank is internally provided with two clapboards for dividing the condensation tank into a first heating area, a second heating area and a third heating area, the pipeline is arranged at the bottom of the first heating area, the two clapboards in the condensation tank are respectively provided with a siphon, wherein the height of the siphon between the first heating area and the second heating area is greater than that between the second heating area and the third heating area, and the temperatures of the first heating area, the second heating area and the third heating area are respectively 80-90 ℃, 130-140 ℃ and 90-100 ℃.
Preferably, return pipes are arranged on the esterification reaction kettle, the first heating zone, the second heating zone and the third heating zone.
Compared with the prior art, the invention has the following implementation effects:
the invention uses the composite catalyst to catalyze the reaction of benzoic acid and methanol, wherein the usage amount of the organic catalyst p-toluenesulfonic acid is only 5-10% of the original single catalyst concentrated sulfuric acid, so that the reversibility of the p-toluenesulfonic acid is improved, the kettle bottom residual liquid containing the catalyst can be recycled, no dangerous waste is generated, and the reaction process is more environment-friendly;
according to the invention, methanol is added below the liquid level, so that the esterification reaction is complete, alkali washing and water washing are not needed, and the rectified methyl benzoate can be directly used for condensation reaction, thereby ensuring continuous production;
the invention takes the dimethylbenzene as a condensation reaction solvent, adds the acetophenone by adopting a mixed mode of the dimethylbenzene and the acetophenone, and simultaneously carries out three times of gradient temperature reactions, thereby improving the reaction speed, shortening the reaction time and improving the yield of the dibenzoyl methane while keeping the concentration of a reaction system in a higher state.
Drawings
FIG. 1 is a schematic diagram of the system of the present invention.
Description of reference numerals: 1. an esterification reaction kettle; 11. an upper feeding pipe; 12. a feeding pipe is arranged; 2. a feed pump; 3. a rectifying tower; 31. a liquid separation plate; 4. a temporary storage tank; 5. a feed tube; 6. a condensation tank; 61. a first heating zone; 62. a second heating zone; 63. a third heating zone; 7. a partition plate; 8. a return pipe.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation to be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1
Taking benzoic acid and methanol as raw materials, wherein the mass ratio of the benzoic acid to the methanol is 1:4, carrying out esterification reaction for 5 hours at 110 ℃ under the catalytic action of a composite catalyst p-toluenesulfonic acid and concentrated sulfuric acid, and rectifying after the reaction is finished to obtain methyl benzoate; wherein the mass of the p-toluenesulfonic acid is 5% of that of the concentrated sulfuric acid, and the addition amount of the composite catalyst is 2% of the total mass of the benzoic acid and the methanol.
Then, directly mixing methyl benzoate with a xylene solution containing acetophenone and sodium methoxide, wherein the mass ratio of the methyl benzoate to the acetophenone is 3:1, the concentrations of the acetophenone and the sodium methoxide in the xylene solution are 53 wt% and 1.6 wt%, mixing, carrying out claisen condensation reaction, carrying out three gradient temperature reactions at 8 ℃, 130 ℃ and 100 ℃, and after the reaction is finished, carrying out acid washing, alkali washing, water washing and crystallization to obtain the dibenzoyl methane.
The continuous dibenzoyl methane preparation system adopted by the preparation method comprises an esterification reaction kettle 1, a rectifying tower 3, a temporary storage tank 4 and a condensation tank 6, wherein the side wall of the esterification reaction kettle 1 is provided with an upper feed pipe 11 and a lower feed pipe 12, the lower feed pipe 12 is arranged below the liquid level in the esterification reaction kettle 1, the bottom of the rectifying tower 3 is connected with the bottom of the esterification reaction kettle 1 through two feed pipes, the lower part of the rectifying tower 3 is provided with a liquid separation plate 31 which divides the bottom of the rectifying tower 3 into a left part and a right part, the feed pipes at the bottom of the rectifying tower 3 are respectively positioned at two sides of the liquid separation plate 31, the top of the rectifying tower 3 is connected with the condensation tank 6 through a pipeline, the temporary storage tank 4 is arranged on the pipeline between the rectifying tower 3 and the condensation tank 6, the pipeline between the temporary storage tank 4 and the condensation tank 6 is also connected with a feed pipe 5, the upper feed pipe 11, the lower feed pipe 12, the feed pipes 5 and the feed pipes between the feed pipes 5 and the temporary storage tank 4 are respectively provided with a feed pump 2, wherein the feeding pumps 2 on the pipelines between the feeding pipes 5 and the temporary storage tank 4 and the feeding pipes 5 adopt chemical metering pumps.
In addition, two clapboards 7 for dividing the condensation tank 6 into a first heating area 61, a second heating area 62 and a third heating area 63 are arranged in the condensation tank 6, a pipeline is arranged at the bottom of the first heating area 61, two clapboards 7 in the condensation tank 6 are respectively provided with a siphon, wherein the height of the siphon between the first heating area 61 and the second heating area 62 is larger than that between the second heating area 62 and the third heating area 63, the temperatures of the first heating area 61, the second heating area 62 and the third heating area 63 are respectively 80 ℃, 130 ℃ and 100 ℃, and return pipes 8 are arranged on the esterification reaction kettle 1, the first heating area 61, the second heating area 62 and the third heating area 63.
When the preparation system is used, the benzoic acid and the methanol are added into an esterification reaction kettle 1, the methanol is added below the liquid level, after esterification reaction, the solution in the esterification reaction kettle 1 is fed into a rectifying tower 3 through one feeding pump 2 between the esterification reaction kettle 1 and the rectifying tower 3 for rectification, the methanol and the benzoic acid are continuously added into the esterification reaction kettle 1, after the esterification reaction is finished again, the solution in the esterification reaction kettle 1 is fed into the rectifying tower 3 through the other feeding pump 2 between the esterification reaction kettle 1 and the rectifying tower 3, meanwhile, the rectified bottom liquid is pumped back into the esterification reaction kettle 1 for reuse, so that the esterification reaction and the rectification can be synchronously carried out, continuous production is realized, the rectified methyl benzoate enters a temporary storage tank 4, passes through a feeding pump 2 and a condensation tank 6, and can be uniformly mixed with a xylene solution containing acetophenone and sodium methoxide in the process of pumping into the condensation tank 6, and simultaneously, the raw materials enter a first heating zone 61, the raw materials are condensed for the first time in the first heating zone 61, the concentration of acetophenone is guaranteed by the first heating zone 61, the reaction efficiency is improved, when the liquid level of the first heating zone 61 reaches the height of a siphon, the solution in the first heating zone 61 can be automatically transferred to a second heating zone 62 for secondary condensation, similarly, after the condensation in the second heating zone 62, the liquid level rises to the top of the siphon between the second heating zone 62 and a third heating zone 63, the solution in the second heating zone 62 enters a third heating zone 63, after the third condensation, a dibenzoyl methane solution is obtained, and finally, the dibenzoyl methane is obtained through acid washing, alkali washing, water washing and crystallization, wherein the yield of dibenzoyl methane can reach 93% and is far higher than the yield of intermittent production, which is 82% based on the dosage of acetophenone.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (6)

1. A continuous preparation method of dibenzoyl methane is characterized by comprising the following steps:
s1, taking benzoic acid and methanol as raw materials, carrying out esterification reaction for 3-6h at the temperature of 100-110 ℃ under the catalytic action of a composite catalyst, and rectifying after the reaction is finished to obtain methyl benzoate;
s2, directly mixing methyl benzoate with a xylene solution containing acetophenone and sodium methoxide, carrying out claisen condensation reaction, and after the reaction is finished, crystallizing and filtering to obtain dibenzoyl methane;
the composite catalyst is a mixture of p-toluenesulfonic acid and concentrated sulfuric acid, wherein the mass of the p-toluenesulfonic acid is 5-10% of that of the concentrated sulfuric acid, and the addition amount of the composite catalyst is 1-3% of the total mass of benzoic acid and methanol.
2. The continuous dibenzoylmethane production process as claimed in claim 1, wherein the ratio of the amounts of benzoic acid and methanol is 1: 4-7.
3. The continuous preparation method of dibenzoylmethane as claimed in claim 1, wherein the claisen condensation reaction is carried out at three temperature gradients of 80-90 ℃, 130-140 ℃ and 90-100 ℃.
4. The system applied to the preparation method according to any one of claims 1 to 3, comprising an esterification reaction kettle, a rectifying tower, a temporary storage tank and a condensation tank, wherein an upper feeding pipe and a lower feeding pipe are arranged on the side wall of the esterification reaction kettle, the lower feeding pipe is arranged below the liquid level in the esterification reaction kettle, the bottom of the rectifying tower is connected with the bottom of the esterification reaction kettle through two feeding pipes, a liquid separating plate for dividing the bottom of the rectifying tower into a left part and a right part is arranged at the lower part of the rectifying tower, the feeding pipes at the bottom of the rectifying tower are respectively positioned at two sides of the liquid separating plate, the top of the rectifying tower is connected with the condensation tank through a pipeline, the temporary storage tank is arranged on the pipeline between the rectifying tower and the condensation tank, a feeding pipe is further connected on the pipeline between the temporary storage tank and the condensation tank, and the upper feeding pipe, the lower feeding pipe is arranged below the liquid level in the esterification reaction kettle, the top of the rectifying tower is connected with the condensation tank through a pipeline, and the temporary storage tank are arranged on the pipeline between the rectifying tower and the condensation tank, And the lower feeding pipe, the conveying pipe, the feeding pipe and the pipeline between the feeding pipe and the temporary storage tank are respectively provided with a feeding pump.
5. The system as claimed in claim 4, wherein the condensation tank is provided with two partitions dividing the condensation tank into a first heating zone, a second heating zone and a third heating zone, the pipe is installed at the bottom of the first heating zone, and the two partitions in the condensation tank are respectively provided with a siphon, wherein the height of the siphon between the first heating zone and the second heating zone is greater than the height of the siphon between the second heating zone and the third heating zone, and the temperatures of the first heating zone, the second heating zone and the third heating zone are respectively 80-90 ℃, 130-140 ℃ and 90-100 ℃.
6. The system of claim 4, wherein return lines are provided in the esterification reaction kettle, the first heating zone, the second heating zone, and the third heating zone.
CN202110707833.1A 2021-06-24 2021-06-24 Continuous preparation method and system of dibenzoylmethane Active CN113620796B (en)

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