CN115403444B - Low-temperature recovery method of tetrachloroethylene in fur dry-cleaning waste - Google Patents

Low-temperature recovery method of tetrachloroethylene in fur dry-cleaning waste Download PDF

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CN115403444B
CN115403444B CN202211094097.8A CN202211094097A CN115403444B CN 115403444 B CN115403444 B CN 115403444B CN 202211094097 A CN202211094097 A CN 202211094097A CN 115403444 B CN115403444 B CN 115403444B
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tetrachloroethylene
dry
solution
water
cleaning waste
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CN115403444A (en
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王亚平
蒋嘉容
赵鸿帅
李书卿
段文文
单思佳
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Jiaxing University
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00Preparation of halogenated hydrocarbons
    • C07C17/38Separation; Purification; Stabilisation; Use of additives
    • C07C17/389Separation; Purification; Stabilisation; Use of additives by adsorption on solids
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00Preparation of halogenated hydrocarbons
    • C07C17/38Separation; Purification; Stabilisation; Use of additives

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Abstract

The invention discloses a low-temperature recovery method of tetrachloroethylene in fur dry-cleaning waste, and relates to the technical field of light industry environmental protection. According to the low-temperature recovery method provided by the invention, the grease-tetrachloroethylene solution is obtained by adding the filter aid into the fur dry-cleaning waste, stirring and dispersing uniformly and then filtering out solid impurities; adding sodium dihydrogen phosphate dihydrate and disodium hydrogen phosphate monohydrate into deionized water to prepare a buffer solution, dissolving lipase by using the buffer solution to obtain a mixed solution, heating the mixed solution to 35-50 ℃, and adding sorbitan monostearate to obtain a lipase aqueous solution; emulsifying the lipase aqueous solution to obtain grease-tetrachloroethylene solution, and catalyzing grease to decompose to obtain a water-in-oil emulsion system; the water and water soluble matters in the water-in-oil emulsion system are removed through dehydration and demulsification of the dry silica gel, tetrachloroethylene is obtained through filtration and separation, and the tetrachloroethylene is recovered at a lower temperature, so that the technical effects of reducing the energy consumption of recovery treatment of tetrachloroethylene in fur dry-cleaning waste and improving the recovery efficiency are achieved.

Description

Low-temperature recovery method of tetrachloroethylene in fur dry-cleaning waste
Technical Field
The invention relates to the technical field of light industry environmental protection, in particular to a low-temperature recovery method of tetrachloroethylene in fur dry-cleaning waste.
Background
In the fur finishing stage of dyed fur and leather blanks, organic solvents are often adopted for degreasing, namely tetrachloroethylene degreasing agents are used for finishing, so that clean and fresh fur is obtained. In dry cleaning machines, as the number of times of recycling tetrachloroethylene increases, the content of grease in tetrachloroethylene becomes higher and higher, and finally, the fluidity of the pasty liquid of grease and tetrachloroethylene becomes worse and the solubility is lowered, so that the dry cleaning function is lost and the grease and tetrachloroethylene have to be discarded. The fur dry-cleaning waste contains a large amount of tetrachloroethylene, belongs to dangerous solid waste (waste class number: HW06; waste code: 900-401-06), needs to be entrusted with special treatment of qualified enterprises, has high treatment cost, and causes the discarding of carbon tetrachloride, and the loss is serious.
The recovery of dry cleaning waste solvents such as tetrachloroethylene mainly adopts an evaporation-condensation recovery method, for example, CN201420499873.7 discloses a dry cleaner for achieving zero discharge of distillation by N times of distillation recovery of tetrachloroethylene. In order to solve the problem of low solvent distillation recovery efficiency in the prior art, an improved scheme is specially provided, wherein an air outlet of an air outlet pipe is arranged at the top of a distillation box; the inlet pipe orifice connecting the diversion pipeline with the machine body is arranged at the lower air inlet of the cooler in the machine; the connecting end of the feedback pipeline and the machine body is arranged at the lower part of the fan; the built-in cooler adopts the refrigeration compressor for refrigeration, optimizes the distillation recovery structure of the dry cleaner, realizes the purpose of zero discharge of tetrachloroethylene distillation through N times of recovery processes of distillation, washing and drying, improves the comfort of the use environment, improves the economic benefit of use and avoids environmental pollution.
In carrying out the present invention, the inventors have found that the related art has at least the following problems:
the existing method for recycling the tetrachloroethylene dry-cleaning waste solvent needs to evaporate the solvent, then condense the solvent to separate and recycle the solvent, the method needs to heat the solvent to the boiling point as a whole, the energy consumption is high, and special equipment is needed for distillation to prevent the tetrachloroethylene from leaking, so that the economic cost of enterprises for recycling is high.
Disclosure of Invention
The invention mainly aims to provide a low-temperature recovery method of tetrachloroethylene in fur dry-cleaning waste, which is used for solving the technical problems of high energy consumption and low efficiency of recovery treatment of tetrachloroethylene in the conventional fur dry-cleaning waste, and achieves the technical effects of reducing the energy consumption of recovery treatment of tetrachloroethylene in the fur dry-cleaning waste and improving the recovery efficiency. The technical scheme of the invention is as follows:
according to an aspect of the embodiment of the present invention, there is provided a method for recycling tetrachloroethylene from dry cleaning waste of pelts at a low temperature, said method comprising:
obtaining fur dry cleaning waste, wherein the fur dry cleaning waste comprises tetrachloroethylene;
adding a filter aid into the fur dry-cleaning waste according to the dosage of 6-16 g/L, stirring and dispersing uniformly, and filtering out solid impurities in the fur dry-cleaning waste to obtain an oil-tetrachloroethylene solution;
adding sodium dihydrogen phosphate dihydrate and disodium hydrogen phosphate monohydrate into deionized water to prepare a buffer solution, dissolving lipase by using the buffer solution to obtain a mixed solution, heating the mixed solution to 35-50 ℃, and adding sorbitan monostearate according to 5-15% of the mixed solution by volume to obtain a lipase aqueous solution, wherein the mass ratio of each component in the mixed solution is that: sodium dihydrogen phosphate dihydrate: disodium phosphate monohydrate: lipase = 100g:2.2g:1.1g: 1-2 g;
maintaining the temperature of 35-50 ℃, adding the lipase aqueous solution to the grease-tetrachloroethylene solution, stirring and reacting for 10-18 h, standing for 2-4 h, and cooling to room temperature to obtain a water-in-oil emulsion system;
adding dry silica gel into the water-in-oil emulsion system, stirring and decoloring for 30min, and filtering and separating to obtain aqueous silica gel and tetrachloroethylene, wherein the tetrachloroethylene is reused for fur dry cleaning.
In a preferred embodiment, the filter aid comprises at least one of kaolin, diatomaceous earth, perlite, cellulose, asbestos, graphite powder, sawdust.
In a preferred embodiment, the method further comprises:
and washing the aqueous silica gel with deionized water for 3-5 times, and drying to obtain dry silica gel, wherein the drying is reused in the next low-temperature recovery method.
In a preferred embodiment, the pH of the buffer solution is adjusted to 7.1-7.3.
In a preferred embodiment, the addition mass of the dry silica gel is 4-8 times the mass of the water phase in the water-in-oil emulsion system.
Compared with the prior art, the low-temperature recovery method of tetrachloroethylene in fur dry-cleaning waste provided by the invention has the following advantages:
according to the low-temperature recovery method of tetrachloroethylene in the fur dry-cleaning waste, the grease-tetrachloroethylene solution is obtained by adding the filter aid into the fur dry-cleaning waste, stirring and dispersing uniformly, and filtering out solid impurities; adding sodium dihydrogen phosphate dihydrate and disodium hydrogen phosphate monohydrate into deionized water to prepare a buffer solution, dissolving lipase by using the buffer solution to obtain a mixed solution, heating the mixed solution to 35-50 ℃, and adding sorbitan monostearate according to 5-15% of the mixed solution by mass part to obtain a lipase aqueous solution; emulsifying the lipase aqueous solution to obtain grease-tetrachloroethylene solution, and catalyzing the decomposition of grease components to obtain a water-in-oil emulsion system; finally, dewatering and demulsifiing by using dry silica gel, removing water and water-soluble matters in the water-in-oil emulsion system, and filtering and separating to obtain tetrachloroethylene, thereby realizing the recovery of tetrachloroethylene in the fur dry-cleaning waste at a lower temperature, and achieving the technical effects of reducing the energy consumption of recovery treatment of tetrachloroethylene in the fur dry-cleaning waste and improving the recovery efficiency.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
Fig. 1 is a process flow diagram illustrating a method for the low temperature recovery of tetrachloroethylene from a pelt dry cleaning waste according to an exemplary embodiment.
Fig. 2 is a schematic view showing a process of a low-temperature recovery method of tetrachloroethylene from dry cleaning waste of pelts according to an exemplary embodiment.
Detailed Description
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only 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.
In the following examples, the lipase was obtained from a lipase preparation of Shenzhen LvWilka Biotechnology Co., ltd, the product number was L0057, the CAS number was 9001-62-1, and the enzyme activity was 5 ten thousand units/g.
The flow chart of the method for recycling tetrachloroethylene in fur dry cleaning waste at low temperature is shown in figure 1, and in figure 1, the method for recycling tetrachloroethylene in fur dry cleaning waste at low temperature specifically comprises the following steps:
step 100: fur dry cleaning waste is obtained, wherein the fur dry cleaning waste comprises tetrachloroethylene.
Step 200: and adding a filter aid into the fur dry-cleaning waste according to the dosage of 6-16 g/L, stirring and dispersing uniformly, and filtering out solid impurities in the fur dry-cleaning waste to obtain the grease-tetrachloroethylene solution.
In a preferred embodiment, the filter aid comprises at least one of kaolin, diatomaceous earth, perlite, cellulose, asbestos, graphite powder, sawdust.
Step 300: adding sodium dihydrogen phosphate dihydrate and disodium hydrogen phosphate monohydrate into deionized water to prepare a buffer solution, dissolving lipase by using the buffer solution to obtain a mixed solution, heating the mixed solution to 35-50 ℃, and adding sorbitan monostearate according to 5-15% of the mixed solution by volume to obtain a lipase aqueous solution, wherein the mass ratio of each component in the mixed solution is that: sodium dihydrogen phosphate dihydrate: disodium phosphate monohydrate: lipase = 100g:2.2g:1.1g: 1-2 g.
In a preferred embodiment, the pH of the buffer solution is adjusted to 7.1-7.3.
Step 400: and (3) adding the lipase aqueous solution to the grease-tetrachloroethylene solution at the temperature of 35-50 ℃, stirring and reacting for 10-18 h, standing for 2-4 h, and cooling to room temperature to obtain the water-in-oil emulsion system.
Tetrachloroethylene is used as a continuous phase in the water-in-oil emulsion system, an aqueous solution is used as a disperse phase, sorbitan monostearate is used as an emulsifier, and lipase in the lipase aqueous solution catalyzes the decomposition of grease components at the oil-water interface of the water-in-oil emulsion system under the continuous stirring at the temperature of 35-50 ℃ and enters into a water phase.
In a preferred embodiment, the addition mass of the dry silica gel is 4-8 times the mass of the water phase in the water-in-oil emulsion system.
Step 500: adding dry silica gel into the water-in-oil emulsion system, stirring and decoloring for 30min, and filtering and separating to obtain aqueous silica gel and tetrachloroethylene, wherein the tetrachloroethylene is reused for fur dry cleaning.
The water and water-soluble matters in the water-in-oil emulsion system can be removed after the dry silica gel is added into the water-in-oil emulsion system, so that the water-in-oil emulsion system is demulsified, the water and water-soluble matters are absorbed by the dry silica gel to form water-containing silica gel, and the remaining liquid tetrachloroethylene is reused for dry cleaning of fur after the water-in-oil emulsion system and the water-in-water soluble matters are simply separated.
In one possible implementation manner, the aqueous silica gel is washed with deionized water for 3-5 times and then dried to obtain dry silica gel, and the dry silica gel is reused in the next low-temperature recovery method.
In one possible embodiment, the invention provides a treatment process schematic diagram of a low-temperature recovery method of tetrachloroethylene in fur dry cleaning waste, which is shown in fig. 2.
Compared with the existing evaporation recovery treatment technology of tetrachloroethylene, the low-temperature recovery method of tetrachloroethylene in the fur dry-cleaning waste provided by the invention can realize separation of grease and tetrachloroethylene at a lower temperature, greatly reduces energy consumption, and in addition, the tetrachloroethylene obtained by separation can be reused for fur dry cleaning, and the water-containing silica gel obtained by separation can be washed and dried to obtain dry silica gel, and the dry silica gel can be continuously reused for the next low-temperature recovery method.
Further, the following specific examples 1 to 3 are exemplified for the application of the method for recovering tetrachloroethylene from fur dry cleaning waste at a low temperature.
Example 1:
step 100: 5L of fur dry cleaning waste including tetrachloroethylene is obtained.
Step 200: adding 30g of kaolin into the fur dry-cleaning waste, stirring and dispersing for 20min, and filtering out solid impurities in the fur dry-cleaning waste to obtain the grease-tetrachloroethylene solution.
Step 300: adding sodium dihydrogen phosphate dihydrate and disodium hydrogen phosphate monohydrate into deionized water to prepare a buffer solution, regulating the pH value of the buffer solution to 7.1, dissolving lipase by using the buffer solution to obtain a mixed solution, heating the mixed solution to 35 ℃, and adding 50g of sorbitan monostearate according to 5% volume part of the mixed solution to obtain a lipase aqueous solution, wherein the mixed solution comprises 100g of deionized water, 2.2g of sodium dihydrogen phosphate dihydrate, 1.1g of disodium hydrogen phosphate monohydrate and 1g of lipase.
Step 400: and (3) adding the aqueous lipase solution to the grease-tetrachloroethylene solution at the temperature of 35 ℃, stirring and reacting for 10 hours, standing for 2 hours, and cooling to room temperature to obtain a water-in-oil emulsion system.
Step 500: adding 600g of dry silica gel into the water-in-oil emulsion system according to 6 times of the mass of the water phase in the water-in-oil emulsion system, stirring and decoloring for 30min, and filtering and separating to obtain the aqueous silica gel and tetrachloroethylene, wherein the tetrachloroethylene is reused for fur dry cleaning. The separated aqueous silica gel was washed with 2kg of deionized water for 3 times and dried for the next dehydration.
Example 2:
step 100: 5L of fur dry cleaning waste including tetrachloroethylene is obtained.
Step 200: adding 40g of kaolin into the fur dry-cleaning waste, stirring and dispersing for 25min, and filtering out solid impurities in the fur dry-cleaning waste to obtain the grease-tetrachloroethylene solution.
Step 300: adding sodium dihydrogen phosphate dihydrate and disodium hydrogen phosphate monohydrate into deionized water to prepare a buffer solution, regulating the pH value of the buffer solution to 7.2, dissolving lipase by using the buffer solution to obtain a mixed solution, heating the mixed solution to 40 ℃, and adding 50g of sorbitan monostearate according to 5% volume part of the mixed solution to obtain a lipase aqueous solution, wherein the mixed solution comprises 100g of deionized water, 2.2g of sodium dihydrogen phosphate dihydrate, 1.1g of disodium hydrogen phosphate monohydrate and 2g of lipase.
Step 400: and (3) adding the aqueous lipase solution to the grease-tetrachloroethylene solution at the temperature of 40 ℃, stirring and reacting for 18 hours, standing for 4 hours, and cooling to room temperature to obtain a water-in-oil emulsion system.
Step 500: adding 600g of dry silica gel into the water-in-oil emulsion system according to 6 times of the mass of the water phase in the water-in-oil emulsion system, stirring and decoloring for 30min, and filtering and separating to obtain the aqueous silica gel and tetrachloroethylene, wherein the tetrachloroethylene is reused for fur dry cleaning. The separated aqueous silica gel was washed with 2kg of deionized water for 3 times and dried for the next dehydration.
Example 3:
step 100: 5L of fur dry cleaning waste including tetrachloroethylene is obtained.
Step 200: adding 80g of kaolin into the fur dry-cleaning waste, stirring and dispersing for 30min, and filtering out solid impurities in the fur dry-cleaning waste to obtain the grease-tetrachloroethylene solution.
Step 300: adding sodium dihydrogen phosphate dihydrate and disodium hydrogen phosphate monohydrate into deionized water to prepare a buffer solution, regulating the pH value of the buffer solution to 7.3, dissolving lipase by using the buffer solution to obtain a mixed solution, heating the mixed solution to 50 ℃, adding 50g of sorbitan monostearate according to 5% volume part of the mixed solution to obtain a lipase aqueous solution, wherein the mixed solution comprises 100g of deionized water, 2.2g of sodium dihydrogen phosphate dihydrate, 1.1g of disodium hydrogen phosphate monohydrate and 2g of lipase.
Step 400: and (3) adding the aqueous lipase solution to the grease-tetrachloroethylene solution at the temperature of 35 ℃, stirring and reacting for 18 hours, standing for 4 hours, and cooling to room temperature to obtain a water-in-oil emulsion system.
Step 500: adding 600g of dry silica gel into the water-in-oil emulsion system according to 6 times of the mass of the water phase in the water-in-oil emulsion system, stirring and decoloring for 30min, and filtering and separating to obtain the aqueous silica gel and tetrachloroethylene, wherein the tetrachloroethylene is reused for fur dry cleaning. The separated aqueous silica gel was washed with 2kg of deionized water for 3 times and dried for the next dehydration.
In summary, the low-temperature recovery method of tetrachloroethylene in fur dry-cleaning waste provided by the invention comprises the steps of adding a filter aid into fur dry-cleaning waste, stirring and dispersing uniformly, and filtering out solid impurities to obtain a grease-tetrachloroethylene solution; adding sodium dihydrogen phosphate dihydrate and disodium hydrogen phosphate monohydrate into deionized water to prepare a buffer solution, dissolving lipase by using the buffer solution to obtain a mixed solution, heating the mixed solution to 35-50 ℃, and adding sorbitan monostearate according to 5-15% of the mixed solution by mass part to obtain a lipase aqueous solution; emulsifying the lipase aqueous solution to obtain grease-tetrachloroethylene solution, and catalyzing the decomposition of grease components to obtain a water-in-oil emulsion system; finally, dewatering and demulsifiing by using dry silica gel, removing water and water-soluble matters in the water-in-oil emulsion system, and filtering and separating to obtain tetrachloroethylene, thereby realizing the recovery of tetrachloroethylene in the fur dry-cleaning waste at a lower temperature, and achieving the technical effects of reducing the energy consumption of recovery treatment of tetrachloroethylene in the fur dry-cleaning waste and improving the recovery efficiency.
While the invention has been described in detail in the foregoing general description, embodiments and experiments, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention herein. This invention is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is to be understood that the invention is not limited to the precise arrangements and instrumentalities shown in the drawings, which have been described above, and that various modifications and changes may be effected without departing from the scope thereof.

Claims (5)

1. A method for the low temperature recovery of tetrachloroethylene from dry cleaning waste of pelts, said method comprising:
obtaining fur dry cleaning waste, wherein the fur dry cleaning waste comprises tetrachloroethylene;
adding a filter aid into the fur dry-cleaning waste according to the dosage of 6-16 g/L, stirring and dispersing uniformly, and filtering out solid impurities in the fur dry-cleaning waste to obtain an oil-tetrachloroethylene solution;
adding sodium dihydrogen phosphate dihydrate and disodium hydrogen phosphate monohydrate into deionized water to prepare a buffer solution, dissolving lipase by using the buffer solution to obtain a mixed solution, heating the mixed solution to 35-50 ℃, and adding sorbitan monostearate according to 5-15% of the mixed solution by volume to obtain a lipase aqueous solution, wherein the mass ratio of each component in the mixed solution is that: sodium dihydrogen phosphate dihydrate: disodium phosphate monohydrate: lipase = 100g:2.2g:1.1g: 1-2 g;
maintaining the temperature of 35-50 ℃, adding the lipase aqueous solution to the grease-tetrachloroethylene solution, stirring and reacting for 10-18 h, standing for 2-4 h, and cooling to room temperature to obtain a water-in-oil emulsion system; adding dry silica gel into the water-in-oil emulsion system, stirring and decoloring for 30min, and filtering and separating to obtain aqueous silica gel and tetrachloroethylene, wherein the tetrachloroethylene is reused for fur dry cleaning.
2. The method of claim 1, wherein the filter aid comprises at least one of kaolin, diatomaceous earth, perlite, cellulose, asbestos, graphite powder, and sawdust.
3. The method according to claim 1, wherein the method further comprises: and washing the aqueous silica gel with deionized water for 3-5 times, and drying to obtain dry silica gel, wherein the dry silica gel is reused in the next low-temperature recovery method.
4. The method of claim 1, wherein the pH of the buffer solution is adjusted to 7.1-7.3.
5. The method according to claim 1, wherein the dry silica gel is added in an amount of 4 to 8 times the mass of the aqueous phase in the water-in-oil emulsion system.
CN202211094097.8A 2022-09-08 2022-09-08 Low-temperature recovery method of tetrachloroethylene in fur dry-cleaning waste Active CN115403444B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5139674A (en) * 1988-12-23 1992-08-18 Novo Nordisk A/S Method of purifying dry-cleaning solvent
CN1433491A (en) * 2000-06-05 2003-07-30 宝洁公司 Domestic fabric article refreshment in integrated cleaning and treatment processes
CN104153163A (en) * 2014-09-01 2014-11-19 郑海通 Dry cleaning machine achieving zero emission of distillation by recycling tetrachloroethylene through N time distillation
CN111056916A (en) * 2019-12-12 2020-04-24 孝感博镧铕新材料有限公司 Method for treating high-boiling-point waste in vinyl chloride production
JP2022077034A (en) * 2020-11-10 2022-05-20 株式会社デジマ Hibiscus hamabo extract, cosmetics containing the hibiscus hamabo extract and functional food

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5139674A (en) * 1988-12-23 1992-08-18 Novo Nordisk A/S Method of purifying dry-cleaning solvent
CN1433491A (en) * 2000-06-05 2003-07-30 宝洁公司 Domestic fabric article refreshment in integrated cleaning and treatment processes
CN104153163A (en) * 2014-09-01 2014-11-19 郑海通 Dry cleaning machine achieving zero emission of distillation by recycling tetrachloroethylene through N time distillation
CN111056916A (en) * 2019-12-12 2020-04-24 孝感博镧铕新材料有限公司 Method for treating high-boiling-point waste in vinyl chloride production
JP2022077034A (en) * 2020-11-10 2022-05-20 株式会社デジマ Hibiscus hamabo extract, cosmetics containing the hibiscus hamabo extract and functional food

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