CN113666821B - High-yield trichloroacetyl chloride preparation system and method - Google Patents
High-yield trichloroacetyl chloride preparation system and method Download PDFInfo
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Abstract
本发明提出的一种高收率三氯乙酰氯制备方法，包括以下步骤：向酰氯混合物通入氯气，发生深度氯化反应，生成三氯乙酰氯；在反应后期，对反应釜内的物质检测成分含量，若酸成分含量高，则向反应釜内加入二氯化二硫，生成的酰氯混合物仍然继续和氯气发生深度氯化反应，生成三氯乙酰氯，本方案在反应釜内反应的过程中，酰氯混合物与氯气深度氯化完毕后，可能残留氯乙酸、二氯乙酸，此时对反应釜内物料成分分析检测，根据检测结果从补充槽内加入二氯化二硫，通过流量阀和控制阀控制二氯化二硫的加入量，进而使酸继续氯化反应完全生成一氯乙酰氯、二氯乙酰氯，再继续被深度氯化，转化为三氯乙酰氯，从而提高三氯乙酰氯的收率。
The invention provides a high-yield trichloroacetyl chloride preparation method, comprising the following steps: introducing chlorine into an acyl chloride mixture to generate trichloroacetyl chloride by deep chlorination reaction; in the later stage of the reaction, detecting the component content of the material in the reactor, if the acid component content is high, adding disulfur dichloride into the reactor, and the generated acyl chloride mixture continues to generate deep chlorination reaction with chlorine to generate trichloroacetyl chloride. In the process of the reaction in the reactor, after the deep chlorination of the acyl chloride mixture and chlorine is completed, chloroacetic acid and dichloroacetic acid may remain. At this time, the material components in the reactor are analyzed and detected, and disulfur dichloride is added from a supplementary tank according to the detection result. The amount of disulfur dichloride added is controlled by a flow valve and a control valve, so that the acid continues to generate monochloroacetyl chloride and dichloroacetyl chloride completely by chlorination reaction, and then continues to be deeply chlorinated to be converted into trichloroacetyl chloride, thereby improving the yield of trichloroacetyl chloride.
Description
Technical Field
The invention relates to the technical field of trichloroacetyl chloride preparation, in particular to a high-yield trichloroacetyl chloride preparation system and method.
Background
Trichloroacetyl chloride is an important intermediate for synthesizing organophosphorus pesticides chlorpyrifos and chlorpyrifos methyl, and most of trichloroacetyl chloride in the market is used for producing chlorpyrifos at present. Chlorpyrifos is an organophosphorus pesticide with high efficiency, broad spectrum, low residue and low drug resistance, and is one of the pesticide varieties with larger production and sales. Along with the forbidden use of 5 high-toxic organophosphorus pesticides such as methamidophos and fipronil, chlorpyrifos becomes one of main alternative varieties. The future market space of trichloroacetyl chloride as chlorpyrifos intermediate is wide.
There are various methods for producing trichloroacetyl chloride, and for example, acetyl chloride or acetaldehyde can be obtained by reacting with chlorine in the presence of activated carbon. The reaction of oxygen with tetrachloroethylene in the presence of ultraviolet light and a catalyst also produces trichloroacetyl chloride. Nitric acid and chloral react to obtain trichloroacetic acid, phosphorus trichloride is added into the trichloroacetic acid to react, and after the reaction is finished, products are separated to obtain trichloroacetyl chloride. And also can be prepared by chloridizing chloroacetic acid waste liquid with chlorine. Then the yield is lower in the existing method for preparing trichloroacetyl chloride by chloridizing chloroacetic acid waste liquid.
Disclosure of Invention
It is necessary to provide a system and a method for preparing trichloroacetyl chloride with high yield.
A high-yield trichloroacetyl chloride preparation system comprises a first reaction kettle, a first condenser, a first gas-liquid separator, a second reaction kettle, a second condenser, a second gas-liquid separator and a supplementing tank, wherein an acyl chloride mixture prepared from chloroacetic acid mother liquor is added into the first reaction kettle, the first reaction kettle is provided with a hole for introducing chlorine, a gas phase outlet of the first reaction kettle is connected with a gas phase inlet of the first condenser, a liquid phase outlet of the first condenser is connected with an inlet of the first gas-liquid separator, a gas phase outlet of the first gas-liquid separator is connected with a supplementing tank, a liquid phase outlet of the first gas-liquid separator is connected with a liquid phase reflux port of the first reaction kettle, an acyl chloride mixture prepared from chloroacetic acid mother liquor is added into the second reaction kettle, the second reaction kettle is provided with a hole for introducing chlorine, a gas phase outlet of the second reaction kettle is connected with a gas phase inlet of the second condenser, a liquid phase outlet of the second condenser is connected with a supplementing tank, a liquid phase outlet of the second gas phase of the second gas-liquid separator is connected with a liquid phase outlet of the second reaction kettle is connected with a liquid phase reflux port of the first reaction kettle, a liquid phase reflux port of the second gas-liquid separator is connected with a second reaction kettle, a second reaction kettle is connected with a first reaction kettle and a second reaction kettle is connected with a second reaction kettle through a second exhaust valve.
A preparation method of high-yield trichloroacetyl chloride comprises the following steps:
Introducing chlorine into the acyl chloride mixture to generate deep chlorination reaction to generate trichloroacetyl chloride, wherein in the step, the main reaction is represented by the equation of the formulas 1-3:
In the later stage of the reaction, detecting the content of components in the substances in the reaction kettle, and if the content of acid components is high, adding disulfide dichloride into the reaction kettle to perform the reaction of the formulas 4-6:
the resultant acid chloride mixture still continues to react with chlorine gas to produce the deep chlorination of formulas 1-3 to produce trichloroacetyl chloride.
The scheme is that two sets of trichloroacetyl chloride reaction kettles are provided with a complementary groove which is used for supplementing disulfide, and the two reaction kettles are respectively controlled by a flow valve and a switch valve. The reaction is continuous for one reaction kettle, namely, the content of substances is detected at the later stage of the reaction, at the moment, the reaction kettle is kept to be filled with chlorine, the detection time is short, in order to fully react the acid substances, direct addition of disulfide is selected instead of sulfur, and if sulfur is added into a supplementing tank, the progress of the reaction of the sulfur and the chlorine and the amount of the generated disulfide cannot be accurately known, and the reaction of the sulfur and the chlorine also requires time, so that direct addition of the disulfide from the supplementing tank is the most preferred scheme. The measurement of the flow valve is adopted, the amount of the dithio dichloride is accurately added into the reaction kettle according to the calculation result, and the purity or the yield of the trichloroacetyl chloride generated by the reaction can reach 99 percent.
In the scheme, after the advanced chlorination of acyl chloride mixture (monochloroacetyl chloride and dichloroacetyl chloride) and chlorine is completed in the reaction process in the reaction kettle, chloroacetic acid and dichloroacetic acid possibly remain, at the moment, the analysis and detection of the components of materials in the reaction kettle are carried out, disulfide is added from the supplementing tank according to the detection result, the addition amount of the disulfide is controlled through the flow valve and the control valve, and then the acid is subjected to continuous chlorination reaction to completely generate monochloroacetyl chloride and dichloroacetyl chloride, and then is subjected to advanced chlorination to be converted into trichloroacetyl chloride, so that the yield of trichloroacetyl chloride is improved.
Drawings
FIG. 1 is a schematic diagram showing the connection of a high-yield trichloroacetyl chloride production system.
FIG. 2 is a schematic diagram showing the connection of a high yield trichloroacetyl chloride production system for another hinge example.
In the figure, a first reaction kettle 10, a first flow valve 11, a first switch valve 12, a first condenser 20, a first gas-liquid separator 30, a second reaction kettle 40, a second flow valve 41, a second switch valve 42, a second condenser 50, a second gas-liquid separator 60, a supplementing tank 70, a feed inlet 71 for adding disulfide, a feed inlet 72 for feeding sulfur, a primary acylating kettle 80 and a vulcanizing kettle 90.
Detailed Description
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Referring to fig. 1, the embodiment of the invention provides a high-yield trichloroacetyl chloride preparation system, which comprises a first reaction kettle 10, a first condenser 20, a first gas-liquid separator 30, a second reaction kettle 40, a second condenser 50, a second gas-liquid separator 60 and a supplementing groove 70, wherein an acyl chloride mixture prepared from chloroacetic acid mother solution is added into the first reaction kettle 10, the first reaction kettle 10 is provided with a hole for introducing chlorine, a gas phase outlet of the first reaction kettle 10 is connected with a gas phase inlet of the first condenser 20, a liquid phase outlet of the first condenser 20 is connected with an inlet of the first gas-liquid separator 30, a gas phase outlet of the first gas-liquid separator 30 is connected with the supplementing groove 70, and a liquid phase outlet of the first gas-liquid separator 30 is connected with a liquid phase reflux port of the first reaction kettle 10; acyl chloride mixture prepared from chloroacetic acid mother liquor is added into the second reaction kettle 40, the second reaction kettle 40 is provided with a hole for introducing chlorine, a gas phase outlet of the second reaction kettle 40 is connected with a gas phase inlet of a second condenser 50, a liquid phase outlet of the second condenser 50 is connected with an inlet of a second gas-liquid separator 60, a gas phase outlet of the second gas-liquid separator 60 is connected with a supplementing groove 70 (unreacted chlorine is recycled into the supplementing groove 70), a liquid phase outlet of the second gas-liquid separator 60 is connected with a liquid phase reflux port of the second reaction kettle 40, the supplementing groove 70 is provided with a port for discharging tail gas and a feed port 71 for adding disulfide, the supplementing groove 70 is also respectively connected with the first reaction kettle 10 and the second reaction kettle 40, a first flow valve 11, a first on-off valve 12 (a metering valve having a flow rate monitoring and on-off control function may be employed), a second flow valve 41, and a second on-off valve 42 are provided between the replenishment tank 70 and the first reaction tank 10 and the second reaction tank 40.
Since monochloroacetyl chloride is also one of the main products produced by the applicant, a large amount of chloroacetic acid mother liquor is generated in the process of preparing monochloroacetyl chloride, and the scheme is to prepare trichloroacetyl chloride by using the chloroacetic acid mother liquor. The method comprises the steps of preparing monochloro-acetyl chloride, namely, firstly, generating dichlorinated disulfide by using chlorine and sulfur, then, reacting acetic acid, dichlorinated disulfide and chlorine to prepare the acyl chloride, separating the acyl chloride by a rectifying tower, generating a large amount of chloroacetic acid mother liquor in the process, then, distilling the chloroacetic acid mother liquor to obtain anhydrous mother liquor, carrying out primary chlorination on the anhydrous chloroacetic acid mother liquor and dichlorinated disulfide to prepare an acyl chloride mixture (mainly, monochloroacetyl chloride, dichlorinated acetyl chloride and incompletely chloroacetic acid, and other impurities which remain in the chloroacetic acid mother liquor or are not fully reacted by the acyl chloride, such as monochloroacetic acid, dichlorinated acetic acid and the like), adding the acyl chloride mixture into a first reaction kettle 10 or a second reaction kettle 40, introducing chlorine, adding a catalyst, and carrying out deep chlorination to obtain trichloroacetyl chloride.
In order to increase the yield of trichloroacetyl chloride, the components of substances in the reaction kettle are detected in the process of the reaction of the first reaction kettle 10 and the second reaction kettle 40, if the detection reaction is finished, chloroacetic acid substances (such as chloroacetic acid and dichloroacetic acid) still remain although the acyl chloride is completely chlorinated, and the substances are mixed in trichloroacyl to lead to low yield of trichloroacetyl chloride, so that the sulfur chloride is added into the supplementing groove 70 according to the consumption of sulfur chloride required to be added according to the detection proportion conversion, chloroacetic acid and dichloroacetic acid are acylated through the supplementing groove 70, and the chlorine is continuously introduced to continue deep chlorination to generate trichloroacetyl chloride, thereby increasing the yield.
This is different from the prior art, and in CN200410021491.4, the process for preparing trichloroacetyl chloride by using chloroacetic acid mother liquor is also disclosed, and part of the processes in this application are the same as those in this application, but there are exactly the problems to be solved in this application, such as that after acylation of chloroacetic acid mother liquor in step b, the mixture of monochloroacetyl chloride and dichloroacetyl chloride is obtained by rectification and separation, and in step c, trichloroacetyl chloride is produced under the action of catalyst pyridine. However, in the step b, the mother solution of chloroacetic acid is refined, and the concept of refining can be explained in two ways, and firstly, if high purity cannot be achieved after refining, acid impurity substances still remain, so that in the process of acyl chlorination, chloroacetic acid cannot completely react due to the existence of no dichlorinated disulfide, and can still remain, and chloroacetic acid or unacylated dichloroacetic acid remains in a mixture of monochloroacetyl chloride and dichloroacetyl chloride, so that the problem solved in the application naturally exists, and the problem is not suggested or solved in the application. Second, if the purification concept is completely high purity, no acid remains, and the technical problem of the present application does not exist. In the same way, the problem also exists in the patent CN201110330108.3, although in claim 3, chloroacetic acid waste liquid is rectified to remove low boiling point substances at 130-140 ℃, and then the mixture of acyl chloride is prepared by catalytic reaction of chlorine and sulfur, however, even if the low boiling point substances are removed, the acyl chlorination reaction of chlorine and chloroacetic acid cannot completely react, then chlorine is introduced into the mixture of acyl chloride and pyridine catalyst is added to generate trichloroacetyl chloride, but because the chloroacetic acid is used as waste liquid, residual chloroacetic acid and dichloroacetic acid are inevitably present in the mixture of generated acyl chloride, the problem of the present application still exists, and if pure mixture of acyl chloride is directly used to prepare trichloroacyl, such as CN2016106822456 and CN201510534467.9, the problem of the present application does not exist, and the present application is not applicable.
Further, the replenishment tank 70 is provided with a feed port 72 into which sulfur is fed.
Referring to fig. 2, the high-yield trichloroacetyl chloride preparation system further comprises a primary acylation kettle 80 and a vulcanization kettle 90, wherein the vulcanization kettle 90 is used for introducing chlorine and adding sulfur to generate disulfide by vulcanization reaction, a discharge outlet of the vulcanization kettle 90 is connected with the primary acylation kettle 80, the primary acylation kettle 80 is used for adding disulfide and distilled anhydrous chloroacetic acid mother liquor to generate primary acylation reaction, monochloroacetyl chloride and dichloroacetyl chloride are mainly generated, and an outlet of the primary acylation kettle 80 is connected with inlets of the first reaction kettle 10 and the second reaction kettle 40.
The invention also provides a preparation method of the high-yield trichloroacetyl chloride, which comprises the following steps:
Introducing chlorine into the acyl chloride mixture to generate deep chlorination reaction to generate trichloroacetyl chloride, wherein in the step, the main reaction is represented by the equation of the formulas 1-3:
In the latter stage of the reaction (for example, the latter 1/3 to 1/2 of the preset reaction time), the content of the components is detected for the substances in the reaction kettle, and if the content of the acid component is high (for example, more than 1%), disulfide is added into the reaction kettle to perform the reaction of the formula 4 to the formula 6:
the resultant acid chloride mixture still continues to react with chlorine gas to produce the deep chlorination of formulas 1-3 to produce trichloroacetyl chloride.
According to the method, the acid substances remained in the later reaction kettle are reacted and converted into acyl chloride mixtures, the acid substances are removed, the reaction kettle is continuously supplied with chlorine, and the acyl chloride mixtures are deeply chlorinated to generate trichloroacetyl chloride.
Further, the preparation method of the high-yield trichloroacetyl chloride is characterized by comprising the following steps of:
In the early reaction stage (for example, the first 1/2-2/3 of the preset reaction time) of the reaction kettle, sulfur is added into the supplementing tank 70, and excessive chlorine in the reaction kettle reacts with the sulfur in the supplementing tank 70 to generate disulfide. The excessive chlorine of the reaction kettle is introduced into the reaction kettle, so that the excessive chlorine of the reaction kettle can be fully utilized, the exhaust system is avoided, the tail gas treatment pressure is reduced, and meanwhile, the utilization rate of the chlorine is high. Meanwhile, the reaction precondition supplementing groove 70 is empty, chlorine is directly discharged after entering, part of sulfur is added into the supplementing groove 70 in the period of time, and the sulfur dichloride can be generated and is supplemented into the reaction kettle when the late stage deep chlorination is carried out. The disulfide is added in the later stage, so that the time of the early reaction can be used for reacting excessive chlorine with sulfur to generate disulfide, the reaction is connected before and after the reaction, and the addition of the disulfide in the supplementing tank 70 can be reduced by supplementing the disulfide in the supplementing tank 70 in a metering mode when the disulfide is added into the reaction kettle in the later stage.
Further, the method comprises the steps of preparing an acyl chloride mixture:
Chlorine and sulfur react in the vulcanizing boiler 90 to generate disulfide, and the main reaction of the step is as follows:
the disulfide is added into an acylation kettle to react with anhydrous chloroacetic acid mother liquor to mainly generate an acyl chloride mixture of acetyl chloride, monochloroacetyl chloride and dichloroacetyl chloride, and the reaction mainly occurs in the step is shown in the formula 4-6.
The modules or units in the device of the embodiment of the invention can be combined, divided and deleted according to actual needs.
The foregoing disclosure is merely illustrative of the presently preferred embodiments of the invention, and it is not intended to limit the scope of the invention, which can be embodied in other specific forms without departing from the spirit or essential characteristics thereof. Those skilled in the art will recognize that the invention can be practiced with modification within the spirit and scope of the appended claims. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (4)
1. The preparation method of the trichloroacetyl chloride with high yield is characterized by comprising the following steps:
Introducing chlorine into the acyl chloride mixture to generate deep chlorination reaction to generate trichloroacetyl chloride, wherein in the step, the main reaction is represented by the equation of the formulas 1-3:
in the later stage of the reaction, detecting the content of components in substances in the reaction kettle, and adding disulfide into the reaction kettle when the content of acid components is high, so as to perform the reactions of the formulas 4-6:
The generated acyl chloride mixture still continues to react with chlorine to generate deep chlorination of the formulas 1-3 to generate trichloroacetyl chloride;
in the early reaction stage of the reaction kettle, adding sulfur into a supplementing tank, and reacting excessive chlorine in the reaction kettle with the sulfur in the supplementing tank to generate disulfide;
the method also comprises the steps of preparing the acyl chloride mixture:
Chlorine and sulfur react in a vulcanizing boiler to generate disulfide, and the main reaction of the step is as follows:
the disulfide is added into an acylation kettle to react with anhydrous chloroacetic acid mother liquor to mainly generate an acyl chloride mixture of acetyl chloride, monochloroacetyl chloride and dichloroacetyl chloride, and the reaction mainly occurs in the step is shown in the formula 4-6.
2. The method for preparing the high-yield trichloroacetyl chloride according to claim 1, wherein the high-yield trichloroacetyl chloride preparation method is realized in a high-yield trichloroacetyl chloride preparation device, the high-yield trichloroacetyl chloride preparation device comprises a first reaction kettle, a first condenser, a first gas-liquid separator, a second reaction kettle, a second condenser, a second gas-liquid separator and a supplementing tank, an acyl chloride mixture prepared from chloroacetic acid mother liquor is added into the first reaction kettle, a hole for introducing chlorine is formed in the first reaction kettle, a gas phase outlet of the first reaction kettle is connected with a gas phase inlet of the first condenser, a liquid phase outlet of the first condenser is connected with an inlet of the first gas-liquid separator, a gas phase outlet of the first gas-liquid separator is connected with the supplementing tank, a liquid phase outlet of the first gas-liquid separator is connected with a liquid phase reflux port of the first reaction kettle, an acyl chloride mixture prepared from chloroacetic acid mother liquor is added into the second reaction kettle, a gas phase outlet of the second reaction kettle is connected with a gas phase inlet of the second condenser, a gas phase outlet of the second condenser is connected with a gas phase inlet of the second condenser, a gas phase outlet of the second gas-liquid separator is connected with a gas phase outlet of the second gas-liquid separator, a gas phase valve of the second reaction kettle is connected with a gas phase outlet of the second reaction kettle, a second gas-phase valve is connected with a second valve of the second reaction kettle is arranged between the second gas-phase outlet of the second reaction kettle, and the first valve is connected with the second valve, and the second valve is connected with the second valve.
3. The method for producing trichloroacetyl chloride with high yield according to claim 2, wherein the replenishing tank is further provided with a feed port for feeding sulfur.
4. The method for preparing high-yield trichloroacetyl chloride according to claim 3, wherein the high-yield trichloroacetyl chloride preparation device further comprises a primary acylation kettle and a vulcanization kettle, wherein the vulcanization kettle is used for introducing chlorine and adding sulfur, a discharge outlet of the vulcanization kettle is connected with the primary acylation kettle, the primary acylation kettle is used for adding dithio dichloride and distilled anhydrous chloroacetic acid mother liquor to perform primary acylation reaction, and monochloroacetyl chloride and dichloroacetyl chloride are mainly generated, and an outlet of the primary acylation kettle is connected with inlets of the first reaction kettle and the second reaction kettle.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106669564A (en) * | 2017-03-21 | 2017-05-17 | 河北东华舰化工有限公司 | Emergency treatment system for chloroacetic acid reaction kettle accidents |
| CN106748739A (en) * | 2015-11-20 | 2017-05-31 | 宁夏际华环境安全科技有限公司 | A kind of trichloro-acetic chloride production technology |
| CN216106704U (en) * | 2021-07-21 | 2022-03-22 | 宁夏荣泰生物科技有限公司 | High-yield trichloroacetyl chloride preparation system |
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| DE2263580C2 (en) * | 1972-12-27 | 1982-06-03 | Basf Ag, 6700 Ludwigshafen | Process for the production of chloroacetyl chloride |
| CN2354958Y (en) * | 1997-08-26 | 1999-12-22 | 陈筱伯 | Apparatus for producing trichlorobenzylidyne |
| CN1562941A (en) * | 2004-03-24 | 2005-01-12 | 大庆市富杰化工有限公司 | Method for preparing trichlorideacetyl chloride from mother liquor of chloroactic acid |
| CN105148710A (en) * | 2015-09-10 | 2015-12-16 | 山东谦诚工贸科技有限公司 | Absorption method of tail gas produced in production of trichloroacetyl chloride by means of chlorination process |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106748739A (en) * | 2015-11-20 | 2017-05-31 | 宁夏际华环境安全科技有限公司 | A kind of trichloro-acetic chloride production technology |
| CN106669564A (en) * | 2017-03-21 | 2017-05-17 | 河北东华舰化工有限公司 | Emergency treatment system for chloroacetic acid reaction kettle accidents |
| CN216106704U (en) * | 2021-07-21 | 2022-03-22 | 宁夏荣泰生物科技有限公司 | High-yield trichloroacetyl chloride preparation system |
Non-Patent Citations (1)
| Title |
|---|
| 氯乙酰氯的合成;林勇等;《化学工程师》;19980626;11-12 * |
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