CN114195667A - Synthesis method of o-trifluoromethyl benzamide - Google Patents

Synthesis method of o-trifluoromethyl benzamide Download PDF

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Publication number
CN114195667A
CN114195667A CN202111440966.3A CN202111440966A CN114195667A CN 114195667 A CN114195667 A CN 114195667A CN 202111440966 A CN202111440966 A CN 202111440966A CN 114195667 A CN114195667 A CN 114195667A
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water
solution
parts
sustained
release
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李全
易观发
郑建章
黎星
杨兆峰
武长福
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Jiangxi Yongtong Technology Co ltd
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Jiangxi Yongtong Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C231/00—Preparation of carboxylic acid amides
    • C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
    • 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
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0052—Preparation of gels
    • B01J13/0065—Preparation of gels containing an organic phase
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12—Naturally occurring clays or bleaching earth
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/12—Powdering or granulating
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/02—Materials undergoing a change of physical state when used
    • C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
    • C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
    • C08J2303/02—Starch; Degradation products thereof, e.g. dextrin
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2401/02—Cellulose; Modified cellulose
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • C08J2405/02—Dextran; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • C08J2405/04—Alginic acid; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds

Abstract

The invention discloses a synthesis method of o-trifluoromethyl benzamide, which comprises the following specific steps: putting ammonia water into a reaction kettle, introducing chilled water into a jacket to control the temperature to be 0-5 ℃, then slowly dropwise adding o-trifluoromethyl benzoyl chloride, adding a gel ball after dropwise adding, stirring for reacting for 6-8h, then stopping the reaction, carrying out solid-liquid separation on a product, allowing liquid to enter a waste water storage tank, and screening a solid product to obtain the o-trifluoromethyl benzamide finished product. The synthesis method of the o-trifluoromethyl benzamide provided by the invention can promote the reaction and comprehensively improve the reaction yield through the process improvement.

Description

Synthesis method of o-trifluoromethyl benzamide
Technical Field
The invention belongs to the technical field of organic synthesis, and particularly relates to a synthesis method of o-trifluoromethyl benzamide.
Background
O-trifluoromethylbenzamide, also known as 2- (trifluoromethyl) benzamide, having the molecular formula C8H6F3NO, molecular weight 189.135, CAS registry number 360-64-5, solid powder at room temperature, melting point 160-164 deg.C, boiling point 247.3 + -40.0 deg.C at 760 mmHg. The o-trifluoromethyl benzamide is a fine organic chemical raw material and an intermediate, and is commonly used for synthesizing amide pesticides, bactericides and other pesticides.
The o-trifluoromethyl benzamide is generally obtained by stirring and reacting o-trifluoromethyl benzoyl chloride and ammonia water at a low temperature, and a solid product can be obtained by filtering, so that the process is simple. However, the synthesis process has the following two problems: firstly, o-trifluoromethyl benzoyl chloride is easy to generate hydrolysis reaction, the existing method for solving the problem is to perform reaction under the condition of low temperature even below zero, but the hydrolysis reaction still exists, and the too low temperature also reduces the reaction activity of o-trifluoromethyl benzoyl chloride; secondly, hydrogen chloride is generated in the reaction, so that an acid-removing agent (alkali) is needed to remove acid, but the strength of the alkali needs to be strictly controlled, otherwise the reaction is easily influenced. Therefore, the yield of the prior synthesis process of the o-trifluoromethyl benzamide is not ideal.
In summary, how to design a synthesis method of o-trifluoromethyl benzamide, which improves the reaction yield by solving the influence of hydrolysis reaction and hydrogen chloride products on the main reaction, is a problem which needs to be solved urgently at present.
Disclosure of Invention
The present invention aims to solve the above problems and provide a method for synthesizing o-trifluoromethyl benzamide, wherein the reaction is promoted by adding gel beads and a slow-release acid-removing agent during the reaction process, thereby comprehensively improving the reaction yield.
The invention realizes the purpose through the following technical scheme, and a method for synthesizing o-trifluoromethyl benzamide comprises the following specific steps:
putting ammonia water into a reaction kettle, introducing chilled water into a jacket to control the temperature to be 0-5 ℃, then slowly dropwise adding o-trifluoromethyl benzoyl chloride, adding a gel ball after dropwise adding, stirring for reacting for 6-8h, then stopping the reaction, carrying out solid-liquid separation on a product, allowing liquid to enter a waste water storage tank, and screening a solid product to obtain the o-trifluoromethyl benzamide finished product.
The gel ball is added in an amount of 1-4% of the mass of ammonia water, and the gel ball is prepared from 5-8 parts of xanthan gum, 3-6 parts of tara gum, 2-3 parts of sodium alginate, 3-5 parts of mica powder, 10-16 parts of cotton fiber and 6-10 parts of calcium bentonite.
Further, the mass concentration of the ammonia water is 20-26%, and the mass ratio of the o-trifluoromethyl benzoyl chloride to the ammonia water is 1: (1.5-2).
Further, the preparation method of the gel ball comprises the following steps:
(1) respectively adding water to xanthan gum and tara gum at 50-60 deg.C to obtain xanthan gum solution and tara gum solution with concentration of 4-8g/L, and adding water to sodium alginate to obtain sodium alginate solution with concentration of 3-5 g/L;
(2) placing the cotton fiber in a cutting machine of 400-1500 r/min to cut into short fiber with the length of 1-3mm, and then placing the short fiber and the calcium bentonite in a dispersion machine of 1000-1500r/min to mix and disperse for 30-60min to obtain short fiber loaded calcium bentonite;
(3) mixing short fiber-loaded calcium bentonite and an adhesive uniformly, putting into a granulator for granulation, sieving with a 60-100 mesh sieve, and drying to obtain fiber granules;
(4) adding fiber particles and mica powder into xanthan gum solution at 70-80 deg.C, mixing, adding sodium alginate solution, stirring for 3-5min, adding tara gum solution dropwise, stirring for 10-20min, standing at room temperature for 2-4 hr to obtain gel, and washing with pure water to obtain gel ball.
Further, the adhesive in the step (3) consists of 10-20 parts of starch adhesive and 3-5 parts of molasses, and the starch adhesive is prepared from the following raw materials: 75-85 parts of water, 14-18 parts of raw starch, 2-6 parts of cooked starch, 0.4-0.6 part of caustic soda and 0.5-0.7 part of borax.
The invention also provides a slow-release acid-forming agent used in the synthesis method of o-trifluoromethyl benzamide, the slow-release acid-forming agent is added into a reaction kettle before the o-trifluoromethyl benzoyl chloride is dripped, and the mass ratio of the slow-release acid-forming agent to the o-trifluoromethyl benzoyl chloride is (1-3): 1.
further, the preparation method of the sustained-release acid-extending agent comprises the following steps:
s1, mixing sodium sulfate, sodium chloride, ammonium chloride and water, heating at 60-80 ℃ for 10-20min, adding a surfactant, and keeping the temperature of the obtained mixed solution for later use;
s2, adding aluminum nitride and aluminum powder into molten polyethylene, uniformly mixing, dropwise adding into the mixed solution obtained in the step S1, standing for 20-40min after dropwise adding, and filtering to obtain solid spheres;
s3, dissolving ethyl cellulose in absolute ethyl alcohol at the temperature of 60-70 ℃, then adding porous ceramic powder and hydrotalcite powder, and uniformly mixing to obtain a membrane preparation solution;
s4, uniformly spraying the film-making liquid on the surface of the solid ball while the liquid is hot, drying the liquid at 80-90 ℃ after the liquid is sprayed, cooling the liquid at room temperature for 1-2h, immersing the obtained material in 10-20 times of sodium carbonate solution at 50-60 ℃ for 2-3h, and evaporating water to obtain the slow-release acid-removing agent.
Further, in step S1, the mass ratio of sodium sulfate, sodium chloride, ammonium chloride to water is 16: 7: 6: 21, the surfactant is lecithin, polysorbate or sodium dodecyl benzene sulfonate.
Further, in the step S2, the mass ratio of the aluminum nitride, the aluminum powder, and the polyethylene is (2-4): (1-2): (40-50), the dropping amount of the three is 40-100 mg/drop.
Further, in step S3, the mass ratio of the ethyl cellulose, the porous ceramic powder, the hydrotalcite powder, and the absolute ethyl alcohol is 1: (1-2): (0.2-0.4): (30-50), wherein the particle size of the porous ceramic powder is 40-80 μm; in step S4, the spraying thickness of the membrane-forming liquid is 0.1-0.3mm, and the mass concentration of the sodium carbonate solution is 20-30%.
The invention also provides the application of the sustained-release deacidification agent in the synthesis method of o-trifluoromethyl benzamide, and the specific steps of screening the solid product are as follows:
uniformly spraying a calcium chloride solution on the surface of the solid product, standing for 20-30min, washing for 1-3 times by pure water at 40-60 ℃, freeze-drying the obtained material under the conditions of (10-20) DEG C and (1.3-5) Pa, then screening by a screening machine, taking the screened material below the screening machine, and drying in vacuum at-0.08 MPa to obtain the calcium chloride-containing solid product.
Wherein the spraying amount of the calcium chloride solution is 0.3-0.8%.
The invention has the beneficial effects that:
(1) because the o-trifluoromethyl benzoyl chloride serving as a reaction raw material is easy to hydrolyze in a water environment, and the concentration of the ammonia water of the system can be gradually reduced in the reaction process of the ammonia water and the o-trifluoromethyl benzoyl chloride, so that the reaction of the o-trifluoromethyl benzoyl chloride and the ammonia is influenced, and the hydrolysis is easy to occur, the gel ball is added into the reaction kettle, and along with the reaction, the gel ball can gradually absorb the redundant water in the reaction liquid, so that the concentration of the ammonia water in the reaction liquid is kept at a higher level, the occurrence of the hydrolysis reaction is reduced, the generation of a target product is promoted, and the reaction yield is improved;
(2) when the gel ball is prepared, the calcium bentonite is loaded by taking the cotton fiber as a carrier, and then the xanthan gum/tara gum/sodium alginate hydrogel is formed on the surface of the gel ball, the hydrogel has hardness and elasticity at low temperature, not only provides a supporting layer for the gel ball, but also has water absorption performance, forms a double-layer water absorption space together with the calcium bentonite layer, has large water absorption capacity, can control the water absorption speed of the gel ball, and can continuously absorb water;
(3) because the calcium bentonite is easy to exchange cations with an external solution, sodium alginate is added when the gel spheres are prepared, sodium ions in the sodium alginate solution are exchanged with calcium ions in the calcium bentonite, and the calcium ions exchanged into the solution can promote the formation of sodium alginate and xanthan hydrogel, so that a primary hydrogel layer can be quickly formed on the surfaces of fiber particles, and the formation of the gel spheres is promoted;
(4) in order to further control the water absorption speed of the gel balls, mica powder is added, and the mica powder can form space blocking in the hydrogel, so that the water absorption speed is reduced, and the influence of the overlarge water absorption speed of the gel balls on the stability of ammonia water is avoided; the molasses is added into the adhesive, so that the molasses is easily dissolved in water, the permeability of the calcium bentonite layer is increased, and a passage is provided for the water absorption of the calcium bentonite layer;
(5) because the synthesis reaction of the invention has hydrogen chloride generation, acid-removing agent is needed to be added to absorb the acid generated by the reaction, but the acid-removing agent is generally alkaline substance, and the main reaction is influenced if the control is not good, the invention adopts the slow-release acid-removing agent, takes sodium carbonate as alkaline component, and achieves the effect of gradually absorbing the hydrogen chloride in the reaction by controlling the release speed of the sodium carbonate, thereby promoting the main reaction;
(6) regarding the form of the acid-removing agent, solid sodium carbonate is selected instead of a sodium carbonate solution, so as to reduce the introduction of moisture and the slow-release effect, but the solubility of the sodium carbonate is very low at low temperature, so that when the slow-release acid-removing agent is prepared, a hydrated salt phase-change material sodium sulfate/sodium chloride/ammonium chloride/water is added inside (the phase-change temperature is about 10 ℃, and overhigh phase-change temperature can cause overhigh heat to influence the temperature of the system), when the slow-release acid-removing agent is added into the system, the internal hydrated salt phase-change material can be gradually solidified to release heat, and then the heat is transferred to the periphery of the slow-release acid-removing agent to promote the dissolution of the sodium carbonate;
(7) when the slow-release acid-forming agent is prepared, the surface of the phase-change material is coated with the polymer containing the heat-conducting materials of aluminum nitride and aluminum powder, so that the heat transfer of the internal phase-change material can be enhanced;
(8) when the sustained-release acid-forming agent is prepared, in the process of coating the phase-change material to prepare the solid ball, the molten polyethylene mixture is directly dripped into the inorganic salt solution, and the dripping amount of the molten polyethylene mixture is controlled to better control the size of the solid ball, so that the size of the sustained-release acid-forming agent is integrally controlled;
(9) when the sustained-release acid-forming agent is prepared, a certain amount of porous ceramic powder is added into a membrane liquid, so that the purpose of loading sodium carbonate can be achieved, and the affinity of the sustained-release acid-forming agent to hydrogen chloride can be increased by adding hydrotalcite powder (which is an alkaline material);
(10) because the target product o-trifluoromethyl benzamide is solid crystalline powder, the gel balls and the slow-release acid-forming agent which are added in the system are mixed with the product, and solid screening is needed; when the product is screened, firstly, a calcium chloride solution is sprayed in, so that calcium chloride reacts with residual ammonium carbonate on the surface of the slow-release acid-forming agent to generate calcium carbonate solid, thereby filling pores on the surface of the slow-release acid-forming agent and preventing powder of a target product from entering the pores to cause product loss during screening; then washing off inorganic salt ions on the surface of the solid product by using pure water, and then carrying out freeze drying and screening in a screening machine, thereby effectively separating out the target product.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Example 1
The embodiment provides a method for synthesizing o-trifluoromethyl benzamide, which comprises the following specific steps:
putting 20% (mass concentration) of ammonia water into a reaction kettle, introducing chilled water into a jacket to control the temperature to be 0 ℃, then slowly dropwise adding o-trifluoromethyl benzoyl chloride, adding a gel ball after dropwise adding, then stirring for reaction for 6 hours, then terminating the reaction, carrying out solid-liquid separation on a product, allowing liquid to enter a waste water storage tank, and screening a solid product to obtain a finished product of o-trifluoromethyl benzamide, wherein the mass ratio of the o-trifluoromethyl benzoyl chloride to the ammonia water is 1: 1.5.
the gel ball is added in an amount of 1% of the mass of ammonia water, and the gel ball is prepared from 5 parts of xanthan gum, 3 parts of tara gum, 2 parts of sodium alginate, 3 parts of mica powder, 10 parts of cotton fiber and 6 parts of calcium bentonite.
The preparation method of the gel ball comprises the following steps:
(1) respectively adding water to xanthan gum and tara gum at 50 ℃ to prepare a xanthan gum solution and a tara gum solution with the concentration of 4g/L, and adding water to sodium alginate to prepare a sodium alginate solution with the concentration of 3g/L for later use;
(2) placing cotton fiber in a cutting machine of 400r/min to cut into short fiber with length of 1mm, and then placing the short fiber and calcium bentonite in a dispersion machine of 1000r/min to mix and disperse for 30min to obtain short fiber-loaded calcium bentonite;
(3) uniformly mixing short fiber-loaded calcium bentonite and an adhesive, putting the mixture into a granulator for granulation, sieving the granules with a 60-mesh sieve, and drying the granules to obtain fiber granules;
(4) adding fiber particles and mica powder into a xanthan gum solution at 70 ℃, uniformly mixing, adding a sodium alginate solution, stirring for 3min, dropwise adding a tara gum solution, stirring for 10min after dropwise adding, standing for 2h at room temperature to obtain a gel, taking out the gel, and washing with pure water to obtain the gel ball.
The adhesive in the step (3) consists of 10 parts of starch adhesive and 3 parts of molasses, and the starch adhesive is prepared from the following raw materials: 75 parts of water, 14 parts of raw starch, 2 parts of cooked starch, 0.4 part of caustic soda and 0.5 part of borax.
Example 2
On the basis of example 1, this embodiment further provides a sustained-release acid-forming agent used in the method for synthesizing o-trifluoromethylbenzamide in example 1, where the sustained-release acid-forming agent is added to the reaction kettle before the o-trifluoromethylbenzoyl chloride is added dropwise, and the mass ratio of the sustained-release acid-forming agent to the o-trifluoromethylbenzoyl chloride is 1: 1.
the preparation method of the sustained-release deacidification agent comprises the following steps:
s1, mixing the components in a mass ratio of 16: 7: 6: 21 mixing sodium sulfate, sodium chloride, ammonium chloride and water, heating at 60 ℃ for 10min, adding lecithin, and keeping the temperature of the obtained mixed solution for later use;
s2, mixing the components in a mass ratio of 2: 1: 40 adding aluminum nitride and aluminum powder into molten polyethylene, uniformly mixing, dropwise adding into the mixed solution obtained in the step S1, wherein the dropwise adding amount is 40 mg/droplet, standing for 20min after dripping, and filtering to obtain solid balls;
s3, dissolving ethyl cellulose in absolute ethyl alcohol at 60 ℃, adding hydrotalcite powder and porous ceramic powder with the particle size of 40 mu m, and uniformly mixing to obtain a membrane preparation liquid, wherein the mass ratio of the ethyl cellulose to the porous ceramic powder to the hydrotalcite powder to the absolute ethyl alcohol is 1: 1: 0.2: 30, of a nitrogen-containing gas;
s4, uniformly spraying the film-making liquid onto the surface of a solid ball while the liquid is hot, wherein the spraying thickness is 0.1mm, drying the liquid at 80 ℃ after the liquid is sprayed, cooling the liquid at room temperature for 1h, immersing the obtained material in 10 times of 20% (mass concentration) sodium carbonate solution at 50 ℃ for 2h, and evaporating water to obtain the slow-release acid-removing agent.
The rest is the same as in example 1.
Example 3
On the basis of embodiment 2, this embodiment also provides an application of the sustained-release friedel-crafts acid agent of embodiment 2 in a synthesis method of o-trifluoromethyl benzamide, and the specific steps of screening the solid product are as follows:
uniformly spraying a calcium chloride solution on the surface of the solid product, wherein the spraying amount is 0.3%, standing for 20min after spraying, washing for 1 time by pure water at 40 ℃, freeze-drying the obtained material at-10 ℃ and 1.3Pa, screening by a screening machine, taking the screened material below the screening machine, and drying in vacuum at-0.08 MPa to obtain the calcium chloride-containing solid product.
The rest is the same as in example 2.
Example 4
The embodiment provides a method for synthesizing o-trifluoromethyl benzamide, which comprises the following specific steps:
adding 23% (mass concentration) of ammonia water into a reaction kettle, introducing chilled water into a jacket to control the temperature to be 3 ℃, then slowly dropwise adding o-trifluoromethyl benzoyl chloride, adding a gel ball after dropwise adding, then stirring for reaction for 7 hours, then terminating the reaction, carrying out solid-liquid separation on the product, allowing liquid to enter a waste water storage tank, and screening the solid product to obtain a finished product of o-trifluoromethyl benzamide, wherein the mass ratio of the o-trifluoromethyl benzoyl chloride to the ammonia water is 1: 1.8.
wherein the addition amount of the gel balls is 2.5 percent of the mass of ammonia water, and the preparation raw materials of the gel balls comprise 6.5 parts of xanthan gum, 4.5 parts of tara gum, 2.5 parts of sodium alginate, 4 parts of mica powder, 13 parts of cotton fiber and 8 parts of calcium bentonite.
The preparation method of the gel ball comprises the following steps:
(1) respectively adding water to xanthan gum and tara gum at 55 ℃ to prepare xanthan gum solution and tara gum solution with the concentration of 6g/L, and adding water to sodium alginate to prepare sodium alginate solution with the concentration of 4g/L for later use;
(2) placing cotton fiber in a cutting machine of 450r/min to cut into short fiber with length of 2mm, and then placing the short fiber and calcium bentonite in a dispersion machine of 1250r/min to mix and disperse for 45min to obtain short fiber-loaded calcium bentonite;
(3) uniformly mixing short fiber-loaded calcium bentonite and an adhesive, putting the mixture into a granulator for granulation, sieving the granules with a 80-mesh sieve, and drying the granules to obtain fiber granules;
(4) adding fiber particles and mica powder into a xanthan gum solution at 75 ℃, uniformly mixing, adding a sodium alginate solution, stirring for 4min, dropwise adding a tara gum solution, stirring for 15min after dropwise adding, standing for 3h at room temperature to obtain a gel, taking out the gel, and washing with pure water to obtain the gel ball.
The adhesive in the step (3) consists of 15 parts of starch adhesive and 4 parts of molasses, and the starch adhesive is prepared from the following raw materials: 80 parts of water, 16 parts of raw starch, 4 parts of cooked starch, 0.5 part of caustic soda and 0.6 part of borax.
The embodiment also provides a sustained-release acid-forming agent used in the synthesis method of o-trifluoromethyl benzamide, wherein the sustained-release acid-forming agent is added into a reaction kettle before the o-trifluoromethyl benzoyl chloride is dropwise added, and the mass ratio of the sustained-release acid-forming agent to the o-trifluoromethyl benzoyl chloride is 2: 1.
the preparation method of the sustained-release deacidification agent comprises the following steps:
s1, mixing the components in a mass ratio of 16: 7: 6: 21 mixing sodium sulfate, sodium chloride, ammonium chloride and water, heating at 70 ℃ for 15min, adding polysorbate, and keeping the obtained mixed solution at a constant temperature for later use;
s2, mixing the components in a mass ratio of 3: 1.5: 45 adding aluminum nitride and aluminum powder into the molten polyethylene, uniformly mixing, dropwise adding the mixture into the mixed solution obtained in the step S1, wherein the dropwise adding amount is 70 mg/drop, standing for 30min after the dropping is finished, and filtering to obtain solid balls;
s3, dissolving ethyl cellulose in absolute ethyl alcohol at 65 ℃, adding hydrotalcite powder and porous ceramic powder with the particle size of 60 mu m, and uniformly mixing to obtain a membrane preparation liquid, wherein the mass ratio of the ethyl cellulose to the porous ceramic powder to the hydrotalcite powder to the absolute ethyl alcohol is 1: 1.5: 0.3: 40;
s4, uniformly spraying the film-making liquid onto the surface of the solid ball while the liquid is hot, wherein the spraying thickness is 0.2mm, drying at 85 ℃ after spraying, cooling at room temperature for 1.5h, immersing the obtained material in 15 times of 25% (mass concentration) sodium carbonate solution at 55 ℃ for 2.5h, and evaporating water to obtain the slow-release acid-forming agent.
The embodiment also provides an application of the sustained-release friedel-crafts acid agent in a synthesis method of o-trifluoromethyl benzamide, and the specific steps of screening a solid product are as follows:
uniformly spraying a calcium chloride solution on the surface of the solid product, wherein the spraying amount is 0.5%, standing for 25min after spraying, washing for 2 times by using pure water at 50 ℃, freeze-drying the obtained material at-15 ℃ and 3Pa, then screening by using a screening machine, taking the screened material below the screening machine, and drying in vacuum at-0.08 MPa to obtain the calcium chloride-containing solid product.
Example 5
The embodiment provides a method for synthesizing o-trifluoromethyl benzamide, which comprises the following specific steps:
putting 26 percent (mass concentration) of ammonia water into a reaction kettle, introducing chilled water into a jacket to control the temperature to be 5 ℃, then slowly dropwise adding o-trifluoromethyl benzoyl chloride, adding a gel ball after dropwise adding, then stirring for reaction for 8 hours, then terminating the reaction, carrying out solid-liquid separation on the product, allowing the liquid to enter a waste water storage tank, and screening the solid product to obtain the o-trifluoromethyl benzamide finished product, wherein the mass ratio of the o-trifluoromethyl benzoyl chloride to the ammonia water is 1: 2.
the gel ball is added in an amount of 4% of the mass of ammonia water, and the gel ball is prepared from 8 parts of xanthan gum, 6 parts of tara gum, 3 parts of sodium alginate, 5 parts of mica powder, 16 parts of cotton fiber and 10 parts of calcium bentonite.
The preparation method of the gel ball comprises the following steps:
(1) respectively adding water to xanthan gum and tara gum at 60 ℃ to prepare xanthan gum solution and tara gum solution with the concentration of 8g/L, and adding water to sodium alginate to prepare sodium alginate solution with the concentration of 5g/L for later use;
(2) placing cotton fiber in a cutting machine of 500r/min to cut into short fiber with length of 3mm, and then placing the short fiber and calcium bentonite in a dispersion machine of 1500r/min to mix and disperse for 60min to obtain short fiber-loaded calcium bentonite;
(3) uniformly mixing short fiber-loaded calcium bentonite and an adhesive, putting the mixture into a granulator for granulation, sieving the granules with a 100-mesh sieve, and drying the granules to obtain fiber granules;
(4) adding fiber particles and mica powder into a xanthan gum solution at 80 ℃, uniformly mixing, adding a sodium alginate solution, stirring for 5min, dropwise adding a tara gum solution, stirring for 20min after dropwise adding, standing for 4h at room temperature to obtain a gel, taking out the gel, and washing with pure water to obtain the gel ball.
The adhesive in the step (3) consists of 20 parts of starch adhesive and 5 parts of molasses, and the starch adhesive is prepared from the following raw materials: 85 parts of water, 18 parts of raw starch, 6 parts of cooked starch, 0.6 part of caustic soda and 0.7 part of borax.
The embodiment also provides a sustained-release acid-forming agent used in the synthesis method of o-trifluoromethyl benzamide, wherein the sustained-release acid-forming agent is added into a reaction kettle before the o-trifluoromethyl benzoyl chloride is dropwise added, and the mass ratio of the sustained-release acid-forming agent to the o-trifluoromethyl benzoyl chloride is 3: 1.
the preparation method of the sustained-release deacidification agent comprises the following steps:
s1, mixing the components in a mass ratio of 16: 7: 6: 21 mixing sodium sulfate, sodium chloride, ammonium chloride and water, heating at 80 ℃ for 20min, adding sodium dodecyl benzene sulfonate, and keeping the temperature of the obtained mixed solution for later use;
s2, mixing the components in a mass ratio of 4: 2: 50, adding aluminum nitride and aluminum powder into molten polyethylene, uniformly mixing, dropwise adding into the mixed solution obtained in the step S1, wherein the dropwise adding amount is 100 mg/drop, standing for 40min after the dropwise adding is finished, and filtering to obtain solid balls;
s3, dissolving ethyl cellulose in absolute ethyl alcohol at 70 ℃, adding hydrotalcite powder and porous ceramic powder with the particle size of 80 microns, and uniformly mixing to obtain a membrane preparation liquid, wherein the mass ratio of the ethyl cellulose to the porous ceramic powder to the hydrotalcite powder to the absolute ethyl alcohol is 1: 2: 0.4: 50;
s4, uniformly spraying the film-making liquid onto the surface of a solid ball while the liquid is hot, wherein the spraying thickness is 0.3mm, drying at 90 ℃ after spraying, cooling at room temperature for 2h, immersing the obtained material in 20 times of 30% (mass concentration) sodium carbonate solution at 60 ℃ for 3h, and evaporating water to obtain the slow-release acid-removing agent.
The embodiment also provides an application of the sustained-release friedel-crafts acid agent in a synthesis method of o-trifluoromethyl benzamide, and the specific steps of screening a solid product are as follows:
uniformly spraying a calcium chloride solution on the surface of the solid product, wherein the spraying amount is 0.8%, standing for 30min after spraying, washing for 3 times by using pure water at 60 ℃, freeze-drying the obtained material at-20 ℃ and 5Pa, then screening by using a screening machine, taking the screened material below the screening machine, and drying in vacuum at-0.08 MPa to obtain the calcium chloride-containing solid product.
Comparative example 1
The comparative example provides a synthesis method of o-trifluoromethyl benzamide, which comprises the following specific steps:
putting 20% (mass concentration) of ammonia water into a reaction kettle, introducing chilled water into a jacket to control the temperature to be 0 ℃, then slowly dropwise adding o-trifluoromethyl benzoyl chloride, adding a gel ball after dropwise adding, then stirring for reaction for 6 hours, then terminating the reaction, carrying out solid-liquid separation on a product, allowing liquid to enter a waste water storage tank, and screening a solid product to obtain a finished product of o-trifluoromethyl benzamide, wherein the mass ratio of the o-trifluoromethyl benzoyl chloride to the ammonia water is 1: 1.5.
comparative example 2
This comparative example differs from example 3 in that the gel beads are added in an amount of 0.5% by mass of the aqueous ammonia.
Comparative example 3
This comparative example differs from example 3 in that the amount of gel beads added was 4.5% by mass of the aqueous ammonia.
Comparative example 4
This comparative example differs from example 3 in that the starting material for the preparation of gel beads does not comprise calcium bentonite, in which case the gel beads are prepared by combining steps (2) and (3) of the process: placing cotton fiber in a cutting machine of 400r/min, cutting into short fiber with length of 1mm, mixing short fiber and binder uniformly, putting into a granulator, granulating, and sieving with a 60-mesh sieve to obtain fiber granules.
Comparative example 5
This comparative example differs from example 3 in that the raw material for the preparation of gel beads does not include cotton fibers, in which case the method for preparing gel beads does not include step (2), and step (3) is: mixing calcium bentonite and adhesive, granulating in a granulator, and sieving with 60 mesh sieve to obtain bentonite granule.
Comparative example 6
This comparative example differs from example 3 in that the starting material for the preparation of gel beads does not include tara gum.
Comparative example 7
This comparative example differs from example 3 in that the starting material for the preparation of the gel beads does not include sodium alginate.
Comparative example 8
The comparative example differs from example 3 in that the raw materials for preparing the gel beads do not include mica powder.
Comparative example 9
This comparative example differs from example 3 in that the process for preparing gel beads comprises the following steps:
(1) respectively adding water to xanthan gum and tara gum at 50 ℃ to prepare a xanthan gum solution and a tara gum solution with the concentration of 4g/L, and adding water to sodium alginate to prepare a sodium alginate solution with the concentration of 3g/L for later use;
(2) placing cotton fibers in a cutting machine of 400r/min to cut the cotton fibers into short fibers with the length of 1mm, then putting the short fibers, calcium bentonite and mica powder into a xanthan gum solution, uniformly mixing, adding a sodium alginate solution, stirring for 3min, then dropwise adding a tara gum solution, stirring for 10min after dripping, then standing for 2h at room temperature to generate a gel, taking out the gel, and washing with pure water to obtain the gel balls.
Comparative example 10
This comparative example differs from example 3 in that the inner calcium bentonite layer and the outer hydrogel layer were exchanged in position, and bentonite spheres were obtained, and the preparation method of the bentonite spheres included the following steps:
(1) respectively adding water to xanthan gum and tara gum at 50 ℃ to prepare a xanthan gum solution and a tara gum solution with the concentration of 4g/L, and adding water to sodium alginate to prepare a sodium alginate solution with the concentration of 3g/L for later use;
(2) at the temperature of 70 ℃, adding mica powder into a xanthan gum solution, uniformly mixing, adding a sodium alginate solution, stirring for 3min, then dropwise adding a tara gum solution, stirring for 10min after dropwise adding, then standing for 2h at room temperature to generate a gel, taking out the gel, and washing with pure water to obtain hydrogel particles;
(3) placing cotton fiber in a cutting machine of 400r/min to cut into short fiber with length of 1mm, and then placing the short fiber and calcium bentonite in a dispersion machine of 1000r/min to mix and disperse for 30min to obtain short fiber-loaded calcium bentonite;
(4) and uniformly mixing the short fiber-loaded calcium bentonite, the hydrogel particles and the adhesive, putting the mixture into a granulator for granulation, sieving the granules with a 60-mesh sieve, and drying the granules to obtain the bentonite balls.
Comparative example 11
This comparative example differs from example 3 in that the raw materials for preparing the gel beads do not include cotton fiber and calcium bentonite, and in this case the method for preparing the gel beads includes the following steps:
(1) respectively adding water to xanthan gum and tara gum at 50 ℃ to prepare a xanthan gum solution and a tara gum solution with the concentration of 4g/L, and adding water to sodium alginate to prepare a sodium alginate solution with the concentration of 3g/L for later use;
(2) at the temperature of 70 ℃, adding mica powder into a xanthan gum solution, uniformly mixing, adding a sodium alginate solution, stirring for 3min, then dropwise adding a tara gum solution, stirring for 10min after dropwise adding, standing for 2h at room temperature to obtain a gel, taking out the gel, and washing with pure water to obtain the gel ball.
Comparative example 12
The comparative example is different from example 3 in that the raw materials for preparing the gel beads do not include xanthan gum, tara gum and sodium alginate, and the gel beads are actually fiber particles at the moment, and the preparation method comprises the following steps:
(1) placing cotton fiber in a cutting machine of 400r/min to cut into short fiber with the length of 1mm, and then placing mica powder, the short fiber and calcium bentonite in a dispersion machine of 1000r/min to mix and disperse for 30min to obtain short fiber loaded calcium bentonite;
(2) and (3) uniformly mixing the short fiber-loaded calcium bentonite and the adhesive, putting the mixture into a granulator for granulation, sieving the granules with a 60-mesh sieve, and drying the granules to obtain fiber granules.
Comparative example 13
This comparative example is different from example 3 in that the binder in the step (3) of preparing gel beads does not include molasses.
Comparative example 14
The comparative example differs from example 4 in that the sustained-release acid-extending agent is directly replaced by a 25% (mass concentration) sodium carbonate solution.
Comparative example 15
The comparative example is different from example 4 in that the sustained-release acid-extending agent does not contain an internal hydrated salt phase-change material, and the preparation method of the sustained-release acid-extending agent comprises the following steps:
s1, mixing the components in a mass ratio of 3: 1.5: 45, adding aluminum nitride and aluminum powder into molten polyethylene, and then extruding and pelletizing to obtain solid balls;
s2, dissolving ethyl cellulose in absolute ethyl alcohol at 65 ℃, adding hydrotalcite powder and porous ceramic powder with the particle size of 60 mu m, and uniformly mixing to obtain a membrane-making solution;
s3, uniformly spraying the film-making liquid onto the surface of the solid ball while the liquid is hot, wherein the spraying thickness is 0.2mm, drying at 85 ℃ after spraying, cooling at room temperature for 1.5h, immersing the obtained material in 15 times of 25% (mass concentration) sodium carbonate solution at 55 ℃ for 2.5h, and evaporating water to obtain the slow-release acid-forming agent.
Comparative example 16
The difference between the comparative example and the example 4 is that the hydrated salt phase-change material in the sustained-release acid-extending agent is replaced by paraffin, namely the step S1 of the preparation method of the sustained-release acid-extending agent is as follows: heating 54 deg.C paraffin for 15min at 70 deg.C, adding polysorbate, and keeping the obtained mixture at a certain temperature for use.
Comparative example 17
The difference between the comparative example and the example 4 is that the step S1 of the preparation method of the sustained-release acid-extending agent is as follows: according to the mass ratio of 16: 7: 6: 21 mixing sodium sulfate, sodium chloride, ammonium chloride and water, heating at 70 ℃ for 15min, adding polysorbate, and refrigerating the obtained mixed solution at-10 ℃ for 3h to obtain a compound hydrated salt crystal;
step S2 is: according to the mass ratio of 3: 1.5: and 45, adding aluminum nitride and aluminum powder into the molten polyethylene, uniformly mixing, spraying to the surface of the composite hydrated salt crystal obtained in the step S1, and curing at room temperature to obtain the solid ball.
Comparative example 18
The present comparative example differs from example 4 in that no polysorbate is added in step S1 of the method for preparing a sustained-release deacidification agent.
Comparative example 19
The difference between the comparative example and example 4 is that no aluminum nitride or aluminum powder is added in step S2 of the preparation method of the sustained-release acid-forming agent.
Comparative example 20
The comparative example is different from example 4 in that the addition amount of the sustained-release acid-providing agent in step S2 is 35 mg/drop.
Comparative example 21
The comparative example is different from example 4 in that the addition amount of the sustained-release acid-providing agent in step S2 is 105 mg/drop.
Comparative example 22
The difference between the comparative example and the example 4 is that no hydrotalcite powder is added in the step S3 of the preparation method of the sustained-release acid-extending agent.
Comparative example 23
The difference between the comparative example and the example 4 is that no porous ceramic powder is added in the step S3 of the preparation method of the sustained-release acid-forming agent.
Comparative example 24
The comparative example is different from example 4 in that the spraying thickness in step S4 of the preparation method of the sustained-release acid-extending agent is 0.1 mm.
Comparative example 25
The comparative example is different from example 4 in that the spraying thickness in step S4 of the method for producing a sustained-release acid-providing agent is 0.4 mm.
Comparative example 26
The difference between the comparative example and the example 4 is that the sodium carbonate solution in the step S4 of the preparation method of the sustained-release acid-extending agent is replaced by potassium carbonate solution.
Comparative example 27
The difference between the comparative example and the example 4 is that the sodium carbonate solution in the step S4 of the preparation method of the sustained-release acid-extending agent is replaced by sodium bicarbonate solution.
Comparative example 28
This comparative example differs from example 5 in that the solid product screening method in the synthesis of o-trifluoromethylbenzamide is: drying the solid product at normal temperature, then sieving the dried solid product in a sieving machine with the sieve pore size of 0.1mm, taking the sieved product below the sieve pore size, and drying the sieved product in vacuum under the pressure of-0.08 MPa to obtain the product.
Comparative example 29
This comparative example differs from example 5 in that the solid product screening method in the synthesis of o-trifluoromethylbenzamide is: washing the solid product with pure water at 60 deg.C for 3 times, freeze drying the obtained material at-20 deg.C under 5Pa, sieving with a sieving machine with sieve pore size of 0.1mm, taking out the sieved material below, and vacuum drying at-0.08 MPa.
Comparative example 30
This comparative example differs from example 5 in that the amount of calcium chloride solution sprayed in the solid product screening step in the synthesis process of o-trifluoromethylbenzamide was 0.2%.
Comparative example 31
This comparative example differs from example 5 in that the amount of calcium chloride solution sprayed in the solid product screening step in the synthesis process of o-trifluoromethylbenzamide was 0.9%.
Firstly, the reaction yield of the invention for synthesizing the o-trifluoromethyl benzamide
Ortho-trifluoromethylbenzamide was synthesized according to the methods of examples 1 to 5 and comparative examples 1 to 31 of the present invention, and the reaction yield, = (actual yield of ortho-trifluoromethylbenzamide/theoretical yield of ortho-trifluoromethylbenzamide) × 100% was calculated after the reaction was completed, and the results are shown in table 1.
TABLE 1
Figure 566371DEST_PATH_IMAGE001
From the results in table 1, it can be seen that the reaction yields of the o-trifluoromethylbenzamides synthesized according to the methods of examples 1 to 5 of the present invention are improved to different degrees, and particularly, the reaction yields of examples 3 to 5 are 95% or more, and the reaction efficiency is high, as compared with comparative example 1 (prior art control). The synthesis method of the present invention can improve the reaction yield.
Compared with the comparative example 1, the gel ball is added into the reaction kettle in the example 1 to absorb excessive moisture, so that the reaction process can be promoted; on the basis of the embodiment 1, the embodiment 2 adds a slow-release acid-forming agent to absorb hydrogen chloride and promote the reaction; however, the presence of gel beads and a sustained-release deacidification agent interferes with the separation of reaction products, and the yield is improved, so that the yield of the embodiment 1 and the embodiment 2 does not greatly increase.
On the basis of the embodiment 2, the embodiment 3 provides a specific product screening method for solving the problem of solid product separation, and as a result, the reaction yield is greatly improved.
Comparative examples 2-13 changed the starting materials and methods for the preparation of gel beads compared to example 3; compared with the example 4, the comparative examples 14 to 27 change the preparation raw materials and the method of the sustained-release acid-extending agent; comparative examples 28-31 changed the solid product sizing process compared to example 5; as a result, the reaction yields of comparative examples 2 to 31 were all reduced to different degrees, indicating that only the process according to the invention gives a comprehensive increase in yield.
The invention has the beneficial effects that: according to the o-trifluoromethyl benzamide provided by the invention, the gel ball and the sustained-release acid-forming agent are added in the reaction process, and the solid product is screened, so that the reaction can be promoted, and the reaction yield is comprehensively improved.
Finally, it should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and not intended to limit the present invention, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or some technical features thereof can be replaced. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A method for synthesizing o-trifluoromethyl benzamide is characterized in that: the method comprises the following specific steps:
putting ammonia water into a reaction kettle, introducing chilled water into a jacket to control the temperature to be 0-5 ℃, then slowly dropwise adding o-trifluoromethyl benzoyl chloride, adding a gel ball after dropwise adding, stirring for reacting for 6-8h, then stopping the reaction, carrying out solid-liquid separation on a product, allowing liquid to enter a waste water storage tank, and screening a solid product to obtain a finished product of o-trifluoromethyl benzamide;
the gel ball is added in an amount of 1-4% of the mass of ammonia water, and the gel ball is prepared from 5-8 parts of xanthan gum, 3-6 parts of tara gum, 2-3 parts of sodium alginate, 3-5 parts of mica powder, 10-16 parts of cotton fiber and 6-10 parts of calcium bentonite.
2. The method for synthesizing o-trifluoromethylbenzamide according to claim 1, characterized in that: the mass concentration of the ammonia water is 20-26%, and the mass ratio of the o-trifluoromethyl benzoyl chloride to the ammonia water is 1: (1.5-2).
3. The method for synthesizing o-trifluoromethylbenzamide according to claim 1, characterized in that: the preparation method of the gel ball comprises the following steps:
(1) respectively adding water to xanthan gum and tara gum at 50-60 deg.C to obtain xanthan gum solution and tara gum solution with concentration of 4-8g/L, and adding water to sodium alginate to obtain sodium alginate solution with concentration of 3-5 g/L;
(2) placing the cotton fiber in a cutting machine of 400-1500 r/min to cut into short fiber with the length of 1-3mm, and then placing the short fiber and the calcium bentonite in a dispersion machine of 1000-1500r/min to mix and disperse for 30-60min to obtain short fiber loaded calcium bentonite;
(3) mixing short fiber-loaded calcium bentonite and an adhesive uniformly, putting into a granulator for granulation, sieving with a 60-100 mesh sieve, and drying to obtain fiber granules;
(4) adding fiber particles and mica powder into xanthan gum solution at 70-80 deg.C, mixing, adding sodium alginate solution, stirring for 3-5min, adding tara gum solution dropwise, stirring for 10-20min, standing at room temperature for 2-4 hr to obtain gel, and washing with pure water to obtain gel ball.
4. The method for synthesizing o-trifluoromethylbenzamide according to claim 3, characterized in that: the adhesive in the step (3) consists of 10-20 parts of starch adhesive and 3-5 parts of molasses, and the starch adhesive is prepared from the following raw materials: 75-85 parts of water, 14-18 parts of raw starch, 2-6 parts of cooked starch, 0.4-0.6 part of caustic soda and 0.5-0.7 part of borax.
5. A sustained-release acid-forming agent used in the method for synthesizing o-trifluoromethylbenzamide as set forth in claim 1, wherein: before dropwise adding o-trifluoromethyl benzoyl chloride, adding a slow-release acid-forming agent into a reaction kettle, wherein the mass ratio of the slow-release acid-forming agent to the o-trifluoromethyl benzoyl chloride is (1-3): 1.
6. the sustained-release deacidification agent according to claim 5, wherein: the preparation method of the sustained-release acid-extending agent comprises the following steps:
s1, mixing sodium sulfate, sodium chloride, ammonium chloride and water, heating at 60-80 ℃ for 10-20min, adding a surfactant, and keeping the temperature of the obtained mixed solution for later use;
s2, adding aluminum nitride and aluminum powder into molten polyethylene, uniformly mixing, dropwise adding into the mixed solution obtained in the step S1, standing for 20-40min after dropwise adding, and filtering to obtain solid spheres;
s3, dissolving ethyl cellulose in absolute ethyl alcohol at the temperature of 60-70 ℃, then adding porous ceramic powder and hydrotalcite powder, and uniformly mixing to obtain a membrane preparation solution;
s4, uniformly spraying the film-making liquid on the surface of the solid ball while the liquid is hot, drying the liquid at 80-90 ℃ after the liquid is sprayed, cooling the liquid at room temperature for 1-2h, immersing the obtained material in 10-20 times of sodium carbonate solution at 50-60 ℃ for 2-3h, and evaporating water to obtain the slow-release acid-removing agent.
7. The sustained-release deacidification agent according to claim 6, wherein: in step S1, the mass ratio of sodium sulfate, sodium chloride, ammonium chloride to water is 16: 7: 6: 21, the surfactant is lecithin, polysorbate or sodium dodecyl benzene sulfonate.
8. The sustained-release deacidification agent according to claim 6, wherein: in the step S2, the mass ratio of the aluminum nitride, the aluminum powder and the polyethylene is (2-4): (1-2): (40-50), the dropping amount of the three is 40-100 mg/drop.
9. The method for synthesizing o-trifluoromethylbenzamide according to claim 8, characterized in that: in step S3, the mass ratio of ethyl cellulose, porous ceramic powder, hydrotalcite powder, and absolute ethyl alcohol is 1: (1-2): (0.2-0.4): (30-50), wherein the particle size of the porous ceramic powder is 40-80 μm; in step S4, the spraying thickness of the membrane-forming liquid is 0.1-0.3mm, and the mass concentration of the sodium carbonate solution is 20-30%.
10. Use of the extended release friedel-crafts agent according to claim 5 in the synthesis process of o-trifluoromethylbenzamide according to claim 1, characterized in that: the screening of the solid product comprises the following specific steps:
uniformly spraying a calcium chloride solution on the surface of the solid product, standing for 20-30min, washing for 1-3 times by pure water at 40-60 ℃, freeze-drying the obtained material under the conditions of (10-20) DEG C and (1.3-5) Pa, then screening by a screening machine, wherein the size of a screen hole is 0.05-0.1mm, taking the screened material below, and drying in vacuum at-0.08 MPa to obtain the calcium chloride-containing solid material;
wherein the spraying amount of the calcium chloride solution is 0.3-0.8%.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101080391A (en) * 2004-12-21 2007-11-28 拜尔农科股份有限公司 Process for the preparation of a 2-pyridylethylcarboxamide derivative
US20170129849A1 (en) * 2014-06-16 2017-05-11 Srf Limited Process for the preparation of 2-(trihalomethyl) benzamide
CN108822024A (en) * 2018-08-28 2018-11-16 陕西恒润化学工业有限公司 A kind of fluopyram and its synthetic method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101080391A (en) * 2004-12-21 2007-11-28 拜尔农科股份有限公司 Process for the preparation of a 2-pyridylethylcarboxamide derivative
US20170129849A1 (en) * 2014-06-16 2017-05-11 Srf Limited Process for the preparation of 2-(trihalomethyl) benzamide
CN108822024A (en) * 2018-08-28 2018-11-16 陕西恒润化学工业有限公司 A kind of fluopyram and its synthetic method

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