CN111470938A - Preparation method of 1,1,1, 3-tetrachloropropane - Google Patents
Preparation method of 1,1,1, 3-tetrachloropropane Download PDFInfo
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- CN111470938A CN111470938A CN202010337171.9A CN202010337171A CN111470938A CN 111470938 A CN111470938 A CN 111470938A CN 202010337171 A CN202010337171 A CN 202010337171A CN 111470938 A CN111470938 A CN 111470938A
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- C07—ORGANIC CHEMISTRY
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- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/26—Preparation of halogenated hydrocarbons by reactions involving an increase in the number of carbon atoms in the skeleton
- C07C17/272—Preparation of halogenated hydrocarbons by reactions involving an increase in the number of carbon atoms in the skeleton by addition reactions
- C07C17/275—Preparation of halogenated hydrocarbons by reactions involving an increase in the number of carbon atoms in the skeleton by addition reactions of hydrocarbons and halogenated hydrocarbons
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- 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
- B01J27/06—Halogens; Compounds thereof
- B01J27/128—Halogens; Compounds thereof with iron group metals or platinum group metals
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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- C—CHEMISTRY; METALLURGY
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2527/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- C07C2527/06—Halogens; Compounds thereof
- C07C2527/128—Compounds comprising a halogen and an iron group metal or a platinum group metal
Abstract
The invention discloses a preparation method of 1,1,1, 3-tetrachloropropane, which comprises the steps of mixing carbon tetrachloride and an auxiliary agent, preheating, forcibly circulating for a period of time, forcibly circulating and reacting with ethylene in an enhanced reactor to obtain a 1,1,1, 3-tetrachloropropane crude product, and finally carrying out rectification under reduced pressure to separate to obtain the 1,1,1, 3-tetrachloropropane. The preparation method of the 1,1,1, 3-tetrachloropropane provided by the invention has the advantages of simple process, low energy consumption and easily controlled reaction process, simultaneously ethylene, carbon tetrachloride and auxiliaries obtained from the top of the first rectifying tower and 75-95% of residual liquid in the kettle of the second rectifying tower can be recycled, the material utilization rate is high, the generation of waste is less, the purity of the prepared target product is high, and meanwhile, an ammonia nitrogen-free and phosphorus-free catalyst is used, so that the pollution problem of three wastes containing nitrogen and phosphorus is solved, and the preparation method is efficient and environment-friendly.
Description
Technical Field
The invention relates to a preparation method of 1,1,1, 3-tetrachloropropane, in particular to a method for preparing 1,1,1, 3-tetrachloropropane by using carbon tetrachloride and ethylene as raw materials.
Background
1,1,1, 3-tetrachloropropane, abbreviated to HCC-250fb, is an important fine chemical which can be used as a paint remover, a degreasing agent and an organic synthetic raw material, for example, for preparing 1-chloro-3, 3, 3-trifluoropropane, 3,3, 3-trifluoropropene or HCC-240 db.
At present, there are various methods for preparing 1,1,1, 3-tetrachloropropane, including a preparation method using ethylene and carbon tetrachloride as raw materials. For example, in 1971, T.Asahara et al discovered that ethylene and carbon tetrachloride could produce 1,1,1, 3-tetrachloropropane, catalyzed by triethyl phosphite-ferric chloride hexahydrate. US4243607 improves the process of t.asahara et al by adding nitrile compounds to trialkyl phosphites and iron salts to synthesize 1,1,1, 3-tetrachloropropane, but with this process the formation of tar by-products is not eliminated. U.S. Pat. No. 2004225166 reports a process for preparing 1,1,1, 3-tetrachloropropane by using iron and tributyl phosphate as catalysts, phosphorus-containing wastewater is easily generated by the process, the environment is polluted, in addition, solid iron powder cannot be effectively dispersed in raw materials in the reaction process, so that the quantitative addition cannot be realized, and the polymerization reaction is easily caused by excessive local catalysts in the reaction process, so that high polymers are increased. Therefore, the traditional 1,1,1, 3-tetrachloropropane synthesis process adopts iron powder, ferric chloride and phosphate system catalyst to regulate the reaction of carbon tetrachloride and chloroethylene, but the use of phosphorus-containing catalyst is easy to generate phosphorus-containing three wastes, the environmental pollution is large, and the post-treatment is difficult; in addition, the used iron powder is easy to agglomerate on the surface of the reactor after reaction and difficult to clean, and the fine iron powder is dispersed in organic high-boiling water, so that the consumption is high, and the separation and the recycling are difficult. Therefore, there is still a need for further improvement in the process for preparing 1,1,1, 3-tetrachloropropane from carbon tetrachloride and ethylene.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the preparation method of the 1,1,1, 3-tetrachloropropane, which is green and environment-friendly, has simple process and is easy to industrialize. In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows: a method for preparing 1,1,1, 3-tetrachloropropane in an intensified reactor by respectively adopting ethanol/phenetole and iron filler to replace phosphate and iron powder mainly comprises the following steps:
(1) preheating the carbon tetrachloride and auxiliary agent mixture, adding the preheated carbon tetrachloride and auxiliary agent mixture into a pipeline strengthening reactor, and performing forced circulation for a period of time;
(2) introducing ethylene into a reinforced reactor to perform forced circulation reaction;
(3) adding the reaction liquid after the forced circulation reaction in the step (2) into a first rectifying tower for rectification, obtaining carbon tetrachloride and an auxiliary agent at the top of the first rectifying tower, and obtaining crude 1,1,1, 3-tetrachloropropane at the bottom of the tower;
(4) adding the crude 1,1,1, 3-tetrachloropropane into a second rectifying tower for high vacuum rectification, obtaining the 1,1,1, 3-tetrachloropropane at the top of the second rectifying tower, and recovering the residual liquid in the tower bottom.
Further, in the step (1), the carbon tetrachloride and the auxiliary agent are uniformly mixed and then preheated to 60-75 ℃, and the forced circulation time of the mixture is 3-6 hours.
Further, the auxiliary agent is ethanol or phenetole, preferably ethanol, and the molar ratio of the auxiliary agent to carbon tetrachloride is 0.005-0.05: 1.
Further, the molar ratio of carbon tetrachloride to ethylene in the step (2) is 1: 1.1-0.9, the forced circulation reaction temperature is 60-90 ℃, and the reaction pressure is 0.5-2.5 MPa.
Further, in the step (2), the ethylene is fully mixed with the liquid material in the Venturi mixer and then is sent into the strengthening reactor.
Further, sampling and analyzing every 0.5h in the reaction process of the step (2), and stopping the reaction when the carbon tetrachloride conversion rate reaches 40-80%.
Furthermore, the reinforced reactors are all pipeline reactors with external pumping circulation, and are filled with iron theta ring packing or iron saddle ring packing or iron pall ring packing, preferably iron theta ring packing, and the packing is stacked into a porous iron packing bed structure.
Further, the temperature of the rectifying tower kettle of the first rectifying tower is 40-60 ℃, and the rectifying pressure is-0.06-0.07 MPa.
Further, ethylene, carbon tetrachloride and an auxiliary agent fraction obtained from the top of the first rectifying tower are recycled to the step (1) for reuse.
Further, the temperature of the rectifying tower kettle of the second rectifying tower is 60-80 ℃, and the rectifying pressure is-0.09 to-0.10 MPa.
Further, 5-25% of the residue in the second rectifying tower is used as a waste liquid discharge system, and 75-95% of the residue is recycled to the step (2).
The invention utilizes hydrogen chloride generated by micro thermal decomposition of materials to continuously wash iron filler filled in a circulating reactor under the action of a circulating pump, and finally generates a ferrous chloride catalyst required by telomerization reaction; the reinforced reactor is adopted, so that the mixing and intermiscibility of gas and liquid phases are enhanced; the solubility of ferrous chloride in a reaction system is increased by adding phenetole or an ethanol auxiliary agent, so that the 1,1,1, 3-tetrachloropropane is prepared in an enhanced reactor. In addition, 75-95% of a certain amount of ferric chloride or ferrous chloride catalyst contained in the residual liquid in the rectifying tower can be used for further improving the telomerization reaction activity in the enhanced reactor, and reducing the discharge of hazardous waste.
Compared with the prior art, the invention has the following beneficial effects:
1) by controlling the conversion rate of the carbon tetrachloride to be 40-80%, the product can be diluted to a certain degree, the decomposition of the product 1,1,1, 3-tetrachloropropane is reduced, and the purity of the finally obtained product is not lower than 99.5%;
2) ethylene, carbon tetrachloride and an auxiliary agent obtained from the top of the first rectifying tower and 75-95% of residual liquid in the kettle of the second rectifying tower can be recycled, the material utilization rate is high, less waste is generated, and the residual liquid in the kettle of the rectifying tower containing a certain amount of ferrous chloride catalyst is used indiscriminately, so that the telomerization reaction activity in the strengthening reactor can be further improved;
3) the porous iron packed bed stacked by the iron theta ring packing or the iron saddle ring packing or the iron pall ring packing is adopted to replace the traditional iron powder, so that the problem that the iron powder is difficult to recycle after reaction is solved, and the large excess iron can reduce a small amount of oxidized ferrous chloride again while slowly releasing a ferrous chloride catalyst, thereby avoiding the high boiling caused by the catalytic decomposition of the material by the ferrous chloride; in addition, the porous iron packed bed with the tightly packed fillers can promote the dispersion of the auxiliary agent, increase the contact area of gas phase and liquid phase, ensure that the reaction is more sufficient, and avoid the adhesion and agglomeration of iron mud on the surface of the reactor after the reaction due to the scouring effect, so that the reactor is easy to clean;
4) ethanol or phenetole is used as an auxiliary agent to replace the traditional phosphate ester substances to be used as a solubilizer of the ferrous chloride, so that the solubility of the washed ferrous chloride catalyst in materials can be increased, the telomerization reaction rate is improved, and the problem of pollution of three wastes containing nitrogen and phosphorus in the traditional process is solved;
5) the gas-liquid mixer with the Venturi mixer is used, so that ethylene and carbon tetrachloride can be fully mixed, the dispersity of ethylene in carbon tetrachloride is greatly improved, the solubility of ethylene in carbon tetrachloride is improved, and the reaction efficiency is improved; in addition, the telomerization reaction of ethylene and carbon tetrachloride is a strong exothermic reaction, and the material decomposition caused by overhigh local reaction temperature is reduced while the dispersibility of reaction materials is improved by using the reinforced reactor.
Drawings
FIG. 1 is a schematic diagram of a process for preparing 1,1,1, 3-tetrachloropropane according to the present invention.
Wherein the reference numerals are: the system comprises a preheating kettle 1, a strengthening reactor 2, a circulating pump 3, a gas-liquid mixer 4, a first rectifying tower 5 and a second rectifying tower 6.
Detailed Description
The present invention is further illustrated by the following examples, but the present invention is not limited to these examples.
Example 1
The strengthening reactor 2 is a pipeline reactor with the internal diameter of 50mm and the length of 32.0m and with an in-vitro pumping circulation, and a porous iron packed bed with iron theta ring packing accumulated is filled inside the pipeline reactor; the preparation process flow of the 1,1,1, 3-tetrachloropropane comprises the following steps:
1) mixing an auxiliary agent (ethanol) and carbon tetrachloride according to a molar ratio of 0.05:1, preheating to 74.6 ℃ in a preheating kettle 1, adding a mixture into a strengthening reactor 2, continuously pumping materials at the upper part of the reactor by using a circulating pump 3, and pumping the materials into the bottom of the strengthening reactor 2 to forcibly and uniformly mix the mixture and circulate for 6 hours;
2) heating the intensified reactor to 89 ℃, arranging a Venturi mixer in a gas-liquid mixer 4, feeding ethylene at a feeding amount of which the molar ratio of ethylene to carbon tetrachloride is 1.09:1.0, fully mixing the ethylene with pumped and circulated liquid materials in the Venturi mixer, adding the ethylene into the intensified reactor 2, controlling the pressure of the reactor to be 1.49MPa, carrying out free radical reaction on iron theta ring fillers, carbon tetrachloride and a small amount of water in a system to generate ferrous chloride (excessive iron fillers and avoid generating the ferric chloride) in the reaction process, using the ferrous chloride as a catalyst to improve the telomerization reaction rate, sampling and analyzing every 0.5h in the reaction process, and stopping the reaction when the conversion rate of the carbon tetrachloride reaches 80%;
3) adding the reaction liquid obtained in the step 2) into a first rectifying tower 5, controlling the temperature of a tower kettle of the first rectifying tower 5 to be 59.7 ℃, controlling the vacuum of the first rectifying tower 5 to be-0.061 MPa, recovering ethylene, carbon tetrachloride and auxiliary agent fractions obtained at the tower top in the rectifying process, and feeding the crude 1,1,1, 3-tetrachloropropane obtained at the tower kettle into a second rectifying tower 6 for high vacuum rectification;
4) controlling the temperature of the tower bottom of the second rectifying tower 6 to be 79.3 ℃, the vacuum of the tower top to be-0.091 MPa, rectifying the crude 1,1,1, 3-tetrachloropropane in the second rectifying tower 6 under high vacuum for 1.5 hours to obtain the 1,1,1, 3-tetrachloropropane at the tower top, wherein the yield is 76 percent, the purity is 99.6 percent, and recovering the residual liquid at the tower bottom.
Example 2
The difference between the embodiment and the embodiment 1 is that ethylene, carbon tetrachloride and an auxiliary agent fraction obtained at the tower top in the step 3) are recycled to the step (1) for reuse, 75-95% of residual liquid in the tower bottom of the second rectifying tower 6 is recycled to the step (2) for reuse, and after the cyclic reaction is carried out once, 1,1,1, 3-tetrachloropropane is finally obtained at the tower top of the second rectifying tower 6, the yield is 78%, and the purity is 99.5%.
Example 3
This example differs from example 1 in that the reaction is carried out without the addition of auxiliary agents, and samples are analyzed in step 2) to find that carbon tetrachloride is not substantially converted.
Example 4
The difference between the embodiment and the embodiment 2 is that in the step 1), the auxiliary agent (ethanol) and the carbon tetrachloride are mixed according to the molar ratio of 0.005:1, the preheating temperature of the mixture is 60.1 ℃, and the mixing time in the strengthening reactor 2 is 3 hours; in the step 2), the temperature of the enhanced reactor 2 is raised to 60.0 ℃, ethylene is introduced into the enhanced reactor 2 for forced circulation reaction at the feeding amount of the molar ratio of ethylene to carbon tetrachloride of 0.9:1.0, the pressure of the reactor is 0.51MPa, samples are taken for analysis every 0.5h in the reaction process, and the reaction is stopped when the conversion rate of carbon tetrachloride reaches 80%; in the step 3), the temperature of the tower bottom 5 of the first rectifying tower is 40.3 ℃, and the rectifying pressure is-0.069 MPa; in the step 4), the temperature of the bottom of the second rectifying tower 6 is 60.2 ℃, the rectifying pressure is-0.10 MPa, and finally the 1,1,1, 3-tetrachloropropane is obtained at the top of the second rectifying tower 6, the yield is 67%, and the purity is 99.6%.
Example 5
The difference between the embodiment and the embodiment 2 is that in the step 1), the molar ratio of the auxiliary agent (ethanol) to the carbon tetrachloride is 0.025:1, the preheating temperature of the mixture is 67.1 ℃, and the mixing time in the strengthening reactor 2 is 4.5 h; in the step 2), the temperature of the enhanced reactor 2 is raised to 75.8 ℃, ethylene is introduced into the enhanced reactor 2 for forced circulation reaction at a feeding amount of the molar ratio of ethylene to carbon tetrachloride of 1.0:1.0, the pressure of the reactor is 1.05MPa, samples are taken every 0.5h for analysis in the reaction process, and the reaction is stopped when the conversion rate of carbon tetrachloride reaches 80%; in the step 3), the temperature of the tower bottom 5 of the first rectifying tower is 50.4 ℃, and the rectifying pressure is-0.066 MPa; in the step 4), the temperature of the tower bottom of the second rectifying tower 6 is 70.5 ℃, the rectifying pressure is-0.095 MPa, and finally the 1,1,1, 3-tetrachloropropane is obtained at the tower top of the second rectifying tower 6, the yield is 72.5 percent, and the purity is 99.6 percent.
Example 6
The difference between the embodiment and the embodiment 2 is that in the step 1), the molar ratio of the auxiliary agent (ethanol) to the carbon tetrachloride is 0.025:1, the preheating temperature of the mixture is 67.3 ℃, and the mixing time in the strengthening reactor 2 is 4.5 h; in the step 2), the temperature of the enhanced reactor 2 is raised to 75.5 ℃, ethylene is introduced into the enhanced reactor 2 for forced circulation reaction at the feeding amount of the molar ratio of ethylene to carbon tetrachloride of 0.9:1.0, the pressure of the reactor is 0.85MPa, samples are taken for analysis every 0.5h in the reaction process, and the reaction is stopped when the conversion rate of carbon tetrachloride reaches 40%; in the step 3), the temperature of the tower bottom 5 of the first rectifying tower is 50.1 ℃, and the rectifying pressure is-0.067 MPa; in the step 4), the temperature of the tower bottom of the second rectifying tower 6 is 70.2 ℃, the rectifying pressure is-0.095 MPa, and finally the 1,1,1, 3-tetrachloropropane is obtained at the tower top of the second rectifying tower 6, the yield is 42.5 percent, and the purity is 99.6 percent.
Example 7
The difference between the embodiment and the embodiment 2 is that a porous iron packed bed stacked by the iron saddle ring packing is filled in the intensified reactor 2, the auxiliary agent is phenetole, the molar ratio of the auxiliary agent (phenetole) to carbon tetrachloride in the step 1) is 0.025:1, the preheating temperature of the mixture is 67.5 ℃, and the mixing time in the intensified reactor 2 is 4.5 hours; in the step 2), the temperature of the enhanced reactor 2 is raised to 75.6 ℃, ethylene is introduced into the enhanced reactor 2 for forced circulation reaction at the feeding amount of the molar ratio of ethylene to carbon tetrachloride of 1.0:1.0, the pressure of the reactor is 1.05MPa, samples are taken for analysis every 0.5h in the reaction process, and the reaction is stopped when the conversion rate of carbon tetrachloride reaches 80%; in the step 3), the temperature of the tower bottom 5 of the first rectifying tower is 50.3 ℃, and the rectifying pressure is-0.066 MPa; in the step 4), the temperature of the bottom of the second rectifying tower 6 is 70.4 ℃, the rectifying pressure is-0.095 MPa, and finally the 1,1,1, 3-tetrachloropropane is obtained at the top of the second rectifying tower 6, the yield is 63.5%, and the purity is 99.7%.
Example 8
The difference between the embodiment and the embodiment 2 is that a porous iron packed bed with iron pall ring packing stacked is filled in the strengthening reactor 2, the auxiliary agent is phenetole, the molar ratio of the auxiliary agent (phenetole) to carbon tetrachloride in the step 1) is 0.025:1, the preheating temperature of the mixture is 67.3 ℃, and the mixing time in the strengthening reactor 2 is 4.5 hours; in the step 2), the temperature of the enhanced reactor 2 is raised to 75.8 ℃, ethylene is introduced into the enhanced reactor 2 for forced circulation reaction at a feeding amount of the molar ratio of ethylene to carbon tetrachloride of 1.0:1.0, the pressure of the reactor is 1.04MPa, samples are taken every 0.5h for analysis in the reaction process, and the reaction is stopped when the conversion rate of carbon tetrachloride reaches 80%; in the step 3), the temperature of the tower bottom 5 of the first rectifying tower is 50.1 ℃, and the rectifying pressure is-0.067 MPa; in the step 4), the temperature of the bottom of the second rectifying tower 6 is 71.5 ℃, the rectifying pressure is-0.094 MPa, and finally the 1,1,1, 3-tetrachloropropane is obtained at the top of the second rectifying tower 6, the yield is 60.6%, and the purity is 99.5%.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-mentioned embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention.
Claims (11)
1. A preparation method of 1,1,1, 3-tetrachloropropane is characterized by mainly comprising the following steps:
(1) preheating the carbon tetrachloride and auxiliary agent mixture, adding the preheated carbon tetrachloride and auxiliary agent mixture into a strengthening reactor, and performing forced circulation for a period of time;
(2) introducing ethylene into a reinforced reactor to perform forced circulation reaction;
(3) adding the reaction liquid after the forced circulation reaction in the step (2) into a first rectifying tower for rectification, obtaining carbon tetrachloride and an auxiliary agent at the top of the first rectifying tower, and obtaining crude 1,1,1, 3-tetrachloropropane at the bottom of the tower;
(4) adding the crude 1,1,1, 3-tetrachloropropane into a second rectifying tower for high vacuum rectification, obtaining the 1,1,1, 3-tetrachloropropane at the top of the second rectifying tower, and recovering the residual liquid in the tower bottom.
2. The method of claim 1, wherein: in the step (1), the carbon tetrachloride and the auxiliary agent are uniformly mixed and then preheated to 60-75 ℃, and the forced circulation time of the mixture is 3-6 hours.
3. The method of claim 2, wherein: the auxiliary agent is ethanol or phenetole, and the molar ratio of the auxiliary agent to carbon tetrachloride is 0.005-0.05: 1.
4. The production method according to claim 3, characterized in that: in the step (2), the ethylene is fully mixed with the liquid material in the Venturi mixer and then is sent into the strengthening reactor.
5. The method of claim 4, wherein: in the step (2), the molar ratio of carbon tetrachloride to ethylene is 1: 1.1-0.9, the forced circulation reaction temperature is 60-90 ℃, and the reaction pressure is 0.5-2.5 MPa.
6. The method of claim 5, wherein: sampling and analyzing every 0.5h in the reaction process of the step (2), and stopping the reaction when the carbon tetrachloride conversion rate reaches 40-80%.
7. The method of claim 6, wherein: the reinforced reactor is a pipeline reactor with an external pumping circulation, iron theta ring packing or iron saddle ring packing or iron pall ring packing is filled in the reinforced reactor, and the packing is stacked into a porous iron packed bed structure.
8. The method of claim 7, wherein: the temperature of the rectifying tower kettle of the first rectifying tower is 40-60 ℃, and the rectifying pressure is-0.06-0.07 MPa.
9. The method of claim 8, wherein: and (3) recycling ethylene, carbon tetrachloride and an auxiliary agent fraction obtained from the top of the first rectifying tower to the step (1) for reuse.
10. The method of claim 9, wherein: the temperature of the rectifying tower kettle of the second rectifying tower is 60-80 ℃, and the rectifying pressure is-0.09 to-0.10 MPa.
11. The method of manufacturing according to claim 10, wherein: and (3) discharging 5-25% of the residual liquid in the second rectifying tower as a waste liquid discharge system, and recycling the residual liquid of 75-95% to the step (2).
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| CN101558031A (en) * | 2006-10-11 | 2009-10-14 | 霍尼韦尔国际公司 | Process for the manufacture of 1,1,1,3,3-pentachloropropane |
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| CN101558031A (en) * | 2006-10-11 | 2009-10-14 | 霍尼韦尔国际公司 | Process for the manufacture of 1,1,1,3,3-pentachloropropane |
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| CN114835554A (en) * | 2021-02-02 | 2022-08-02 | 中国科学院宁波材料技术与工程研究所 | Preparation method of 1,1,1, 3-tetrachloropropane |
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