CN112939730A - Hexachlorocyclopentadiene front fraction recycling treatment process and device - Google Patents
Hexachlorocyclopentadiene front fraction recycling treatment process and device Download PDFInfo
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- CN112939730A CN112939730A CN202110135518.6A CN202110135518A CN112939730A CN 112939730 A CN112939730 A CN 112939730A CN 202110135518 A CN202110135518 A CN 202110135518A CN 112939730 A CN112939730 A CN 112939730A
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- C07—ORGANIC CHEMISTRY
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- 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
- C07—ORGANIC CHEMISTRY
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Abstract
The invention discloses a hexachlorocyclopentadiene front cut recycling process and a device, wherein hexachlorocyclopentadiene front cut is added into an alkali washing kettle for heat preservation and stirring, and simultaneously, a sodium hydroxide solution is dropwise added, then, the mixture is kept stand, and a lower organic phase is introduced into a preheating kettle; and then preheating operation is carried out, the outlet end at the top end of the rectifying tower is closed, the preheated material is fed into the rectifying tower kettle, the temperature of the rectifying tower kettle is adjusted, the vacuum degree of the rectifying tower is controlled, hexachloroethane is extracted from the hexachloroethane extraction port until the hexachloroethane is extracted, the hexachloroethane extraction port is closed, the outlet end at the top end of the rectifying tower is opened, hexachlorobutadiene is enriched by utilizing the reflux of the tower top buffer tank, and the separated hexachlorocyclopentadiene is collected through the hexachlorocyclopentadiene receiving tank. Thereby increasing the content of hexachlorocyclopentadiene extracted from hexachlorocyclopentadiene front cut fraction and realizing effective resource utilization.
Description
Technical Field
The invention relates to the technical field of chemical raw material treatment, in particular to a hexachlorocyclopentadiene front-cut recycling treatment process and device.
Background
Hexachlorocyclopentadiene is an important chemical raw material and can be used for synthesizing pesticides, medicines and polyurethane flame retardants, hexachlorocyclopentadiene forms aromatic pentachlorocyclopentadiene anions, so that hexachlorocyclopentadiene has active property and can generate Diels-Alder reaction with most dienophiles, and the conditions are mild, and the temperature is generally between 20 and 200 ℃; even with simple olefins, polycyclic aromatic hydrocarbons (e.g., naphthalene, anthracene, etc.) that are unreactive under normal conditions. Hexachlorocyclopentadiene is used as an intermediate for producing pesticides, and is used for producing organochlorine insecticides and acaricides, such as mirex, aldrin, dieldrin, chlordane, endosulfan and the like, before the 60 th century. Hexachlorocyclopentadiene is also used as a flame retardant and a curing agent for polyester resins and polyurethane foams. As the downstream products of hexachlorocyclopentadiene are more, the market demand is large, and the economic benefit is better.
In the existing hexachlorocyclopentadiene production process, dicyclopentadiene is cracked into cyclopentadiene monomers, the cyclopentadiene monomers react with chlorine to generate tetrachlorocyclopentane, the tetrachlorocyclopentane is deeply chlorinated to generate hexachlorocyclopentylene, and the hexachlorocyclopentadiene finished product is dechlorinated and rectified, but a front fraction of about 8% is generated in the post-treatment rectification separation process of a hexachlorocyclopentadiene device, wherein the hexachlorocyclopentadiene content is 70% -80%, the hexachlorobutadiene content is 15% -20%, and the hexachloroethane content is 5% -10%, and after endosulfan is prohibited from being produced at the end of 3 months in 2018, the front fraction which is used for producing endosulfan before has no good way to be exported, or is treated as dangerous waste or temporarily stored. The waste is treated as hazardous waste, and the treatment requirement and the cost are very high; as a temporary inventory, it also bears a significant safety and environmental risk, and will eventually be disposed of as hazardous waste.
In the existing extraction method for hexachlorocyclopentadiene in hexachlorocyclopentadiene front cut fraction, the content of hexachlorocyclopentadiene extracted is low, and the recycling treatment of hexachlorocyclopentadiene in hexachlorocyclopentadiene front cut fraction can not be realized.
Disclosure of Invention
The invention aims to provide a hexachlorocyclopentadiene front fraction recycling treatment process and a hexachlorocyclopentadiene front fraction recycling treatment device, and aims to solve the technical problems that in a hexachlorocyclopentadiene front fraction hexachlorocyclopentadiene extraction method in the prior art, the content of hexachlorocyclopentadiene extracted is low, and the hexachlorocyclopentadiene front fraction recycling treatment cannot be realized.
In order to achieve the purpose, the hexachlorocyclopentadiene front-fraction recycling treatment device comprises an alkaline washing kettle, a preheating kettle, a rectifying tower, a hexachlorocyclopentadiene receiving tank, a tower top buffer tank, a hexachlorocyclopentadiene receiving tank and a hexachlorobutadiene receiving tank, wherein the discharge end of the alkaline washing kettle is communicated with the feed end of the preheating kettle, the discharge end of the preheating kettle is communicated with the feed end of the rectifying tower kettle, the rectifying tower is provided with a hexachloroethane extraction port, the hexachlorocyclopentadiene extraction port is communicated with the hexachlorocyclopentadiene receiving tank, the top end of the rectifying tower kettle is communicated with the bottom end of the rectifying tower, the top end of the rectifying tower is communicated with the tower top buffer tank, and the tower top buffer tank is respectively communicated with the hexachlorocyclopentadiene receiving tank, the hexachlorobutadiene receiving tank.
The invention also provides a hexachlorocyclopentadiene front cut recycling treatment process adopting the hexachlorocyclopentadiene front cut recycling treatment device, which comprises the following steps:
adding hexachlorocyclopentadiene front fraction into an alkaline washing kettle, keeping the temperature, stirring, simultaneously dropwise adding a sodium hydroxide solution, standing, and introducing a lower-layer organic phase into the preheating kettle;
after the lower organic phase enters the preheating kettle, preheating operation is carried out, the outlet end at the top end of the rectifying tower is closed at the same time, the preheated material is fed to the rectifying tower kettle, then the temperature of the rectifying tower kettle is adjusted, the vacuum degree of the rectifying tower is controlled at the same time, and hexachloroethane is extracted from a hexachloroethane extraction outlet;
and detecting the content of the extracted hexachloroethane after the feeding is finished, closing the hexachloroethane extraction outlet until the hexachloroethane extraction is finished, opening the outlet end at the top end of the rectifying tower, refluxing and enriching hexachlorobutadiene by using the tower top buffer tank, collecting the hexachlorobutadiene through the hexachlorobutadiene receiving tank, and collecting the separated hexachlorocyclopentadiene through the hexachlorocyclopentadiene receiving tank.
Wherein, in the step of dropwise adding a sodium hydroxide solution and then standing: 5% -10% of sodium hydroxide solution is dripped, and the PH value is controlled to be 7-8.
Wherein, in the step of dropwise adding a sodium hydroxide solution and then standing: standing for 30-50 min.
Wherein, after the lower organic phase enters the preheating kettle, the preheating operation is carried out in the following steps: the preheating temperature is 65-80 ℃.
Wherein, in the steps of feeding the preheated material to the rectifying tower kettle, then adjusting the temperature of the rectifying tower kettle, and simultaneously controlling the vacuum degree of the rectifying tower: and adjusting the temperature of the rectifying tower kettle to be 150-180 ℃.
The invention has the beneficial effects that: adding hexachlorocyclopentadiene front fraction into an alkaline washing kettle, keeping the temperature, stirring, simultaneously dropwise adding a sodium hydroxide solution, standing, and introducing a lower-layer organic phase into the preheating kettle; after the lower organic phase enters the preheating kettle, preheating operation is carried out, the outlet end at the top end of the rectifying tower is closed at the same time, the preheated material is fed to the rectifying tower kettle, then the temperature of the rectifying tower kettle is adjusted, the vacuum degree of the rectifying tower is controlled at the same time, and hexachloroethane is extracted from a hexachloroethane extraction outlet; and detecting the content of the extracted hexachloroethane after the feeding is finished, closing the hexachloroethane extraction outlet until the hexachloroethane extraction is finished, opening the outlet end at the top end of the rectifying tower, refluxing and enriching hexachlorobutadiene by using the tower top buffer tank, collecting the hexachlorobutadiene through the hexachlorobutadiene receiving tank, and collecting the separated hexachlorocyclopentadiene through the hexachlorocyclopentadiene receiving tank. Thereby increasing the content of hexachlorocyclopentadiene extracted from hexachlorocyclopentadiene front cut fraction and realizing effective resource utilization.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of the steps of example 1 of the present invention.
Fig. 2 is a flowchart of the steps of embodiment 2 of the present invention.
Fig. 3 is a flowchart of the steps of embodiment 3 of the present invention.
FIG. 4 is a schematic diagram of a recycling apparatus for hexachlorocyclopentadiene front cut according to the present invention.
1-a front fraction tank, 2-an alkali tank, 3-an alkali washing kettle, 4-a preheating kettle, 5-a rectifying tower, 6-a rectifying tower kettle, 7-a heat exchanger, 8-a hexachloroethane condenser, 9-a hexachloroethane receiving tank, 10-a tower top condenser, 11-a tower top buffer tank, 12-a hexachlorocyclopentadiene receiving tank, 13-a hexachlorobutadiene receiving tank, 14-a hexachloroethane extraction outlet, 15-an outlet, 16-a backflow pipe, 17-a discharge pipe, 18-an insertion pipe and 19-a discharge valve.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1 to 4, the invention provides a recycling treatment device for hexachlorocyclopentadiene front-cut, comprising an alkaline washing kettle 3, a preheating kettle 4, a rectifying tower kettle 6, a rectifying tower 5, a hexachloroethane receiving tank 9, a tower top buffer tank 11, a hexachlorocyclopentadiene receiving tank 12 and a hexachlorobutadiene receiving tank 13, the discharge end of the alkaline washing kettle 3 is communicated with the feed end of the preheating kettle 4, the discharge end of the preheating kettle 4 is communicated with the feed end of the rectifying tower kettle 6, the rectifying tower 5 is provided with a hexachloroethane extraction outlet 14, the hexachloroethane extraction outlet 14 is communicated with the hexachloroethane receiving groove 9, the top end of the rectifying tower kettle 6 is communicated with the bottom end of the rectifying tower 5, the top end of the rectifying tower 5 is communicated with the top buffer tank 11, the tower top buffer tank 11 is respectively communicated with the hexachloroethane receiving tank 9, the hexachlorocyclopentadiene receiving tank 12 and the hexachlorobutadiene receiving tank 13.
The recycling treatment device for the hexachlorocyclopentadiene front-cut fraction further comprises a front-cut fraction tank 1 and an alkali tank 2, wherein the front-cut fraction tank 1 and the alkali tank 2 are respectively communicated with the alkali washing kettle 3.
The hexachlorocyclopentadiene front-cut recycling device further comprises a heat exchanger 7 and a hexachloroethane condenser 8, wherein one end of the heat exchanger 7 is communicated with the hexachloroethane extraction port 14, the other end of the heat exchanger 7 is communicated with one end of the hexachloroethane condenser 8, and the other end of the hexachloroethane condenser 8 is communicated with the hexachloroethane receiving tank 9.
The hexachlorocyclopentadiene front-cut recycling device further comprises an overhead condenser 10, wherein one end of the overhead condenser 10 is communicated with the top end of the rectifying tower 5, and the other end of the overhead condenser 10 is communicated with the overhead buffer tank 11.
The hexachloroethane extraction outlet 14 is positioned at 15-40% of the lower part of the rectifying tower 5.
The rectification tower 5 is internally provided with any one of Raschig ring packing, pall ring packing, step ring packing and rectangular saddle packing, the rectification tower 5 is internally distributed by a weir disc type distributor, and the number of the distributors is 10-15.
The bottom of top of the tower buffer tank 11 is provided with two exports 15, hexachlorocyclopentadiene front cut resourceful treatment device still includes back flow pipe 16, discharging pipe 17, insert tube 18 and discharge valve 19, the one end of back flow pipe 16 with one of them of top of the tower buffer tank 11 export 15 intercommunication, the other end of back flow pipe 16 with rectifying column 5 intercommunication, the one end and another of insert tube 18 export 15 intercommunication, just insert tube 18 insert to the degree of depth of top of the tower buffer tank 11 is 40cm-50cm, the other end of insert tube 18 with discharge valve 19 intercommunication, discharge valve 19 with discharging pipe 17 intercommunication.
In the present embodiment, the front cut tank 1 is used for containing hexachlorocyclopentadiene front cut, and the alkali tank 2 is used for containing sodium hydroxide solution. The hexachloroethane extraction outlet 14 is positioned at 15-40% of the lower part of the rectifying tower 5, wherein the lower 20% of the rectifying tower 5 is preferred; the rectification tower 5 is internally provided with any one of Raschig ring packing, pall ring packing, step ring packing and saddle packing, and the rectification tower 5 is internally distributed by a weir-disk distributor with 10-15 layers, preferably 12 layers. Adding hexachlorocyclopentadiene front fraction in the front fraction tank 1 into the preheating kettle 4, dropwise adding a sodium hydroxide solution in the alkali tank 2 under the conditions of heat preservation and open stirring of the preheating kettle 4, controlling the pH value to be 7-8, standing for 30-50 min, taking a lower organic phase, putting the lower organic phase into the preheating kettle 4, controlling the preheating temperature to be 65-80 ℃, controlling the outlet end at the top end of the rectifying tower 5 to be closed after the preheating temperature is up, feeding the preheated material into the rectifying tower kettle 6, continuously feeding the preheated material into the rectifying tower kettle 6 from the preheating kettle 4 for 0.3L/h-0.5L/h, adjusting the temperature of the rectifying tower kettle 6 to be 150-180 ℃, simultaneously controlling the vacuum degree of the rectifying tower 5, extracting hexachloroethane from the hexachlorocyclopentadiene extraction outlet 14, and detecting the content of the extracted material after the feeding is finished, and after the hexachloroethane is extracted, adjusting the material discharged from the tower to the material discharged from the top of the tower, refluxing and enriching hexachlorobutadiene through a buffer tank 11 at the top of the tower, sampling and analyzing every 50-70 min until the hexachlorobutadiene is completely separated, and adjusting the material to be extracted when the hexachlorocyclopentadiene content is increased to more than 98.5%. Thereby increasing the content of hexachlorocyclopentadiene extracted from hexachlorocyclopentadiene front cut fraction and realizing effective resource utilization. Compared with the hexachlorocyclopentadiene front cut fraction in the prior art, the main reason that the effective hexachlorocyclopentadiene content is always high is that the hexachlorocyclopentadiene front cut fraction mainly comprises hexachlorocyclopentadiene, hexachlorobutadiene and hexachloroethane, the three substances are mutually soluble, in the rectifying column 5, since hexachloroethane is vaporized first due to its relatively low volatility, when the hexachloroethane content exceeds 20%, the problem that hexachloroethane is condensed and desublimated on the walls of 17 discharge pipes and 10 tubes of the tower top condenser to form white crystals, the system is blocked seriously, the rectification process cannot be continued, and the pipes and equipment blocked by hexachloroethane solid are not easy to be dredged quickly can be solved, so that the problems that the tower top condenser 10, the hexachloroethane extraction outlet 14 and the discharge pipes 17 are easy to block in the rectification process of the hexachlorocyclopentadiene front cut can be solved.
The invention also provides a hexachlorocyclopentadiene front cut recycling treatment process adopting the hexachlorocyclopentadiene front cut recycling treatment device, which comprises the following steps:
adding hexachlorocyclopentadiene front fraction into an alkaline washing kettle 3, keeping the temperature, stirring, simultaneously dropwise adding a sodium hydroxide solution, standing, and introducing a lower-layer organic phase into a preheating kettle 4;
after the lower organic phase enters the preheating kettle 4, preheating operation is carried out, the outlet end at the top end of the rectifying tower 5 is closed, the preheated material is fed to the rectifying tower kettle 6, then the temperature of the rectifying tower kettle 6 is adjusted, the vacuum degree of the rectifying tower 5 is controlled, and hexachloroethane is extracted from the hexachloroethane extraction outlet 14;
and after the feeding is finished, detecting the content of the extracted hexachloroethane, closing the hexachloroethane extraction outlet 14 until the hexachloroethane extraction is finished, opening the outlet end at the top end of the rectifying tower 5, refluxing and enriching hexachlorobutadiene by using the tower top buffer tank 11, collecting the hexachlorobutadiene through the hexachlorobutadiene receiving tank 13, and collecting the separated hexachlorocyclopentadiene through the hexachlorocyclopentadiene receiving tank 12.
In the step of dropwise adding a sodium hydroxide solution, followed by standing: 5% -10% of sodium hydroxide solution is dripped, and the PH value is controlled to be 7-8.
In the step of dropwise adding a sodium hydroxide solution, followed by standing: standing for 30-50 min.
After the lower organic phase enters the preheating kettle 4, the preheating operation is carried out: the preheating temperature is 65-80 ℃.
In the steps of feeding the preheated material to the rectifying tower kettle 6, then adjusting the temperature of the rectifying tower kettle 6, and simultaneously controlling the vacuum degree of the rectifying tower 5: the temperature of the rectifying tower kettle 6 is adjusted to be 150-180 ℃.
In the steps of feeding the preheated material to the rectifying tower kettle 6, then adjusting the temperature of the rectifying tower kettle 6, and simultaneously controlling the vacuum degree of the rectifying tower 5: the vacuum degree of the rectifying tower 5 is controlled to be-0.095 MPa-0.1 MPa.
In the step of reflux-enriching hexachlorobutadiene using the overhead buffer tank 11: sampling and analyzing the collected hexachlorobutadiene every 50-70 min until the hexachlorobutadiene is completely separated.
Referring to fig. 1, embodiment 1, a hexachlorocyclopentadiene front cut recycling process includes the following steps:
s1: adding 1L of hexachlorocyclopentadiene front fraction into an alkaline washing kettle 3, keeping the temperature, stirring, simultaneously dropwise adding a 5% sodium hydroxide solution, controlling the pH value to be 7, standing for 30min, taking a lower-layer organic phase, and introducing the lower-layer organic phase into a preheating kettle 4;
s2: after the lower organic phase enters the preheating kettle 4, preheating operation with the preheating temperature of 65 ℃ is carried out, the outlet end at the top end of the rectifying tower 5 is closed, the preheated material is continuously fed into the rectifying tower kettle 6 for 0.3L/h, then the temperature of the rectifying tower kettle 6 is adjusted to 150 ℃, the vacuum degree of the rectifying tower 5 is controlled to be-0.095 MPa, and hexachloroethane is extracted from the hexachloroethane extraction outlet 14;
s3: and after the feeding is finished, detecting the content of the extracted hexachloroethane, closing the hexachloroethane extraction outlet 14 until the hexachloroethane extraction is finished, opening the outlet end at the top end of the rectifying tower 5, utilizing the overhead buffer tank 11 to reflux and enrich hexachlorobutadiene, sampling and analyzing every 50min until the hexachlorobutadiene is completely separated, collecting the hexachlorobutadiene through the hexachlorobutadiene receiving tank 13, and collecting the separated hexachlorocyclopentadiene through the hexachlorocyclopentadiene receiving tank 12.
Referring to fig. 2, embodiment 2, a hexachlorocyclopentadiene front cut recycling process includes the following steps:
s1: adding 1L of hexachlorocyclopentadiene front fraction into an alkaline washing kettle 3, keeping the temperature, stirring, simultaneously dropwise adding a 10% sodium hydroxide solution, controlling the pH value to be 8, standing for 50min, taking a lower-layer organic phase, and introducing the lower-layer organic phase into a preheating kettle 4;
s2: after the lower organic phase enters the preheating kettle 4, preheating operation with the preheating temperature of 80 ℃ is carried out, the outlet end at the top end of the rectifying tower 5 is closed, the preheated material is continuously fed into the rectifying tower kettle 6 for 0.5L/h, then the temperature of the rectifying tower kettle 6 is adjusted to 180 ℃, the vacuum degree of the rectifying tower 5 is controlled to be-0.1 MPa, and hexachloroethane is extracted from the hexachloroethane extraction outlet 14;
s3: and after the feeding is finished, detecting the content of the extracted hexachloroethane, closing the hexachloroethane extraction outlet 14 until the hexachloroethane extraction is finished, opening the outlet end at the top end of the rectifying tower 5, utilizing the overhead buffer tank 11 to reflux and enrich hexachlorobutadiene, sampling and analyzing every 70min until the hexachlorobutadiene is completely separated, collecting the hexachlorobutadiene through the hexachlorobutadiene receiving tank 13, and collecting the separated hexachlorocyclopentadiene through the hexachlorocyclopentadiene receiving tank 12.
Referring to fig. 3, embodiment 3, a hexachlorocyclopentadiene front cut recycling process includes the following steps:
s1: adding 1L of hexachlorocyclopentadiene front fraction into an alkaline washing kettle 3, keeping the temperature, stirring, simultaneously dropwise adding 8% sodium hydroxide solution, controlling the pH value to be 7.5, standing for 40min, taking a lower-layer organic phase, and introducing the lower-layer organic phase into a preheating kettle 4;
s2: after the lower organic phase enters the preheating kettle 4, preheating operation is carried out at the preheating temperature of 70 ℃, the outlet end at the top end of the rectifying tower 5 is closed, the preheated material is continuously fed into the rectifying tower kettle 6 for 0.4L/h, then the temperature of the rectifying tower kettle 6 is adjusted to 165 ℃, the vacuum degree of the rectifying tower 5 is controlled to be-0.098 MPa, and hexachloroethane is extracted from the hexachloroethane extraction outlet 14;
s3: and after the feeding is finished, detecting the content of the extracted hexachloroethane, closing the hexachloroethane extraction outlet 14 until the hexachloroethane extraction is finished, opening the outlet end at the top end of the rectifying tower 5, utilizing the overhead buffer tank 11 to reflux and enrich hexachlorobutadiene, sampling and analyzing every 60min until the hexachlorobutadiene is completely separated, collecting the hexachlorobutadiene through the hexachlorobutadiene receiving tank 13, and collecting the separated hexachlorocyclopentadiene through the hexachlorocyclopentadiene receiving tank 12.
In summary, the following steps: the hexachlorocyclopentadiene front cut recycling treatment process and the device can extract hexachlorocyclopentadiene finished products with higher content from hexachlorocyclopentadiene front cut, and realize effective recycling utilization. And simultaneously effectively solves the problems of pipeline blockage and the like in the recycling process of hexachlorocyclopentadiene front-cut.
Claims (6)
1. A hexachlorocyclopentadiene front fraction resourceful treatment device, which is characterized in that,
the device comprises an alkaline washing kettle, a preheating kettle, a rectifying tower, a hexachlorocyclopentadiene receiving groove, a tower top buffer tank, a hexachlorocyclopentadiene receiving groove and a hexachlorobutadiene receiving groove, wherein the discharge end of the alkaline washing kettle is communicated with the feed end of the preheating kettle, the discharge end of the preheating kettle is communicated with the feed end of the rectifying tower kettle, the rectifying tower is provided with a hexachloroethane extraction port, the hexachloroethane extraction port is communicated with the hexachloroethane receiving groove, the top end of the rectifying tower kettle is communicated with the bottom end of the rectifying tower, the top end of the rectifying tower is communicated with the tower top buffer tank, and the tower top buffer tank is respectively communicated with the hexachloroethane receiving groove, the hexachlorocyclopentadiene receiving groove and the hexachlorobutadiene receiving groove.
2. The recycling treatment process of hexachlorocyclopentadiene front cut by adopting the recycling treatment device of hexachlorocyclopentadiene front cut as claimed in claim 1, characterized by comprising the following steps:
adding hexachlorocyclopentadiene front fraction into an alkaline washing kettle, keeping the temperature, stirring, simultaneously dropwise adding a sodium hydroxide solution, standing, and introducing a lower-layer organic phase into the preheating kettle;
after the lower organic phase enters the preheating kettle, preheating operation is carried out, the outlet end at the top end of the rectifying tower is closed at the same time, the preheated material is fed to the rectifying tower kettle, then the temperature of the rectifying tower kettle is adjusted, the vacuum degree of the rectifying tower is controlled at the same time, and hexachloroethane is extracted from a hexachloroethane extraction outlet;
and detecting the content of the extracted hexachloroethane after the feeding is finished, closing the hexachloroethane extraction outlet until the hexachloroethane extraction is finished, opening the outlet end at the top end of the rectifying tower, refluxing and enriching hexachlorobutadiene by using the tower top buffer tank, collecting the hexachlorobutadiene through the hexachlorobutadiene receiving tank, and collecting the separated hexachlorocyclopentadiene through the hexachlorocyclopentadiene receiving tank.
3. The process for recycling a hexachlorocyclopentadiene front fraction as recited in claim 2, wherein in the step of dropping a sodium hydroxide solution and then standing: 5% -10% of sodium hydroxide solution is dripped, and the PH value is controlled to be 7-8.
4. The process for recycling a hexachlorocyclopentadiene front fraction as recited in claim 2, wherein in the step of dropping a sodium hydroxide solution and then standing: standing for 30-50 min.
5. The process for recycling the hexachlorocyclopentadiene front fraction as recited in claim 2, wherein the preheating operation is carried out after the lower organic phase enters the preheating kettle, and the preheating operation comprises the following steps: the preheating temperature is 65-80 ℃.
6. The recycling process of hexachlorocyclopentadiene front-cut according to claim 2, wherein in the step of feeding the preheated material to the bottom of said rectifying tower, then adjusting the temperature of the bottom of said rectifying tower and simultaneously controlling the vacuum degree of said rectifying tower: and adjusting the temperature of the rectifying tower kettle to be 150-180 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB771856A (en) * | 1954-07-16 | 1957-04-03 | Pechiney Prod Chimiques Sa | Improvements in or relating to the production of hexachlorocyclopentadiene |
| US3996112A (en) * | 1971-11-01 | 1976-12-07 | Hooker Chemicals & Plastics Corporation | Distillation of hexahalocyclopentadiene |
| CN102942442A (en) * | 2012-11-27 | 2013-02-27 | 四川大学 | Method for purifying hexachlorocyclopentadiene |
-
2021
- 2021-02-01 CN CN202110135518.6A patent/CN112939730A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB771856A (en) * | 1954-07-16 | 1957-04-03 | Pechiney Prod Chimiques Sa | Improvements in or relating to the production of hexachlorocyclopentadiene |
| US3996112A (en) * | 1971-11-01 | 1976-12-07 | Hooker Chemicals & Plastics Corporation | Distillation of hexahalocyclopentadiene |
| CN102942442A (en) * | 2012-11-27 | 2013-02-27 | 四川大学 | Method for purifying hexachlorocyclopentadiene |
Non-Patent Citations (1)
| Title |
|---|
| 尚颖: "全级戊环癸烷的研制" * |
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