CN106673055A - Method for recycling waste mercury catalyst from polyvinyl chloride production based on calcium carbide method - Google Patents
Method for recycling waste mercury catalyst from polyvinyl chloride production based on calcium carbide method Download PDFInfo
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- CN106673055A CN106673055A CN201611149476.7A CN201611149476A CN106673055A CN 106673055 A CN106673055 A CN 106673055A CN 201611149476 A CN201611149476 A CN 201611149476A CN 106673055 A CN106673055 A CN 106673055A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G13/00—Compounds of mercury
- C01G13/04—Halides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28073—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being in the range 0.5-1.0 ml/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4893—Residues derived from used synthetic products, e.g. rubber from used tyres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Catalysts (AREA)
Abstract
The invention provides a method for recycling a waste mercury catalyst from polyvinyl chloride production based on a calcium carbide method. The method comprises the following steps: smashing the waste mercury catalyst with mercuric chloride, hydrogen chloride and vinyl chloride attached to activated carbon into certain fineness; extracting with carbon disulfide and filtering, thereby acquiring filter residues; heating and then condensing the filter residues under a light-shielding condition to recycle mercuric chloride; treating the filter residues with alkali, neutralizing the absorbed hydrogen chloride, filtering, drying and recycling the activated carbon. The recycling method provided by the invention has the advantages that the heating temperature for recycling the mercuric chloride is low, the recycling of the mercuric chloride can be carried out only at 90-120 DEG C, the recovery rate reaches up to 95% and the purity reaches up to 99.5%; after the recycled activated carbon is treated, the purity is high, the recovery rate reaches up to 92%, the absorption activity is recovered, the micro-pore surface area is recovered to 1000-1200m<2>/g and the pore volume is recovered to 0.3-0.6ml/g; besides, according to the method, the operation is simple, the energy consumption is low, the environment-friendly and pollution-free effects are achieved; the organic substances, such as chloroethylene, and the hydrogen chloride acidic material can be effectively removed.
Description
Technical field
The present invention relates to catalyst reclaims field, and in particular to give up mercury catalyst in a kind of generated by polyvinyl chloride by calcium carbide production
Recovery method.
Background technology
In generated by polyvinyl chloride by calcium carbide production process, acetylene and hydrogen chloride are adopted for raw material, mercuric chloride and activated carbon are to urge
Agent, carries out catalytic reaction and carrys out synthesis vinyl chloride thereof monomer, and then polymerization of vinyl choride monomer forms polrvinyl chloride.With catalytic reaction
Carrying out, easily the Hg chloride content of distillation is reduced to less than 4% in activated carbon, while because having adsorbed excess in activated carbon hole
Raw material hydrogen chloride gas and product vinyl chloride, catalyst gradually inactivates.With China to environmental protection requirement it is increasingly strict, it is primary
State hydrargyrum resource is fewer and feweri, needs to reclaim useless mercury catalyst.The mercury catalyst that gives up in prior art is reclaimed typically will be useless
The mercury catalyst first steaming and decocting together with lime water, makes mercuric chloride be converted into mercury oxide, then Jing 700-800 DEG C high temperature makes mercury oxide become single
Matter hydrargyrum, this kind of method response rate is low by only 57% or so, and energy consumption is big；Also have and poisonous chlorine time is passed through in heating process
Hydrargyrum and mercuric chloride are received, last gas from dry distillation tail causes mercury-containing waste water, pollutes environment again after processing；It is not right in prior art in addition
The organic substance and hydrochloric acid material of activated carbon adsorption is effectively removed, and affects the quality for reclaiming material.
Therefore, these problems how to be solved, it has also become those skilled in the art's technical barrier urgently to be resolved hurrily.
The content of the invention
The present invention is directed to the deficiencies in the prior art, there is provided hydrargyrum catalysis of giving up in a kind of generated by polyvinyl chloride by calcium carbide production
The recovery method of agent, solves above-mentioned technical problem.
To achieve these goals, the present invention provides following technical scheme：Give up hydrargyrum in a kind of generated by polyvinyl chloride by calcium carbide production
The recovery method of catalyst, comprises the steps：
（1）First useless mercury catalyst is crushed to into certain fineness, the useless hydrargyrum catalysis system refers to and be adsorbed with activated carbon mercuric chloride, chlorination
The decaying catalyst of hydrogen and vinyl chloride；
（2）Useless mercury catalyst after by above-mentioned crushing removes vinyl chloride with extraction with carbon disulfide, is filtrated to get filtering residue；
（3）Above-mentioned filtering residue is heated under the conditions of lucifuge and obtains chlorination mercuryvapour, mercuric chloride solid is reclaimed in then condensation；
（4）By remaining filtering residue alkali process after above-mentioned recovery mercuric chloride, the hydrogen chloride of absorption is neutralized, filtered, be dried, reclaimed and live
Property charcoal.
As a further improvement on the present invention, step（1）Described in give up mercury catalyst in be respectively 2- containing mass fraction
The vinyl chloride of 3.8% mercuric chloride, the hydrogen chloride of 0.5-1% and 0.1-0.4%.
As a further improvement on the present invention, step（1）Described in give up mercury catalyst crush after fineness be 40-80 mesh,
The contact area of useless mercury catalyst and extractant Carbon bisulfide can be increased, other Organic substances such as vinyl chloride of absorption in activated carbon
It is easier to be dissolved in Carbon bisulfide；More preferably 60 mesh, fineness blocks filter opening when easily causing filtration more than 80 mesh, and fineness is little
In 40 mesh, Organic substance vinyl chloride is not high by extraction with carbon disulfide rate.
As a further improvement on the present invention, step（2）Described in give up mercury catalyst be with Carbon bisulfide mass volume ratio
1：1.5-3, more preferably 1:2.2, make useless mercury catalyst be easier to be infiltrated by Carbon bisulfide, and extract dosage properly, save
Resource.
As a further improvement on the present invention, step（3）Described under the conditions of lucifuge heating-up temperature be 90-120 DEG C, plus
The hot time is 30-120min, makes mercuric chloride rapid sublimation, reclaims rapid, and lucifuge condition can avoid mercuric chloride from being partially converted into
Calomel, the response rate is up to 95%, reclaims product purity and is up to 99.5%.
As a further improvement on the present invention, step（3）Described in condensation temperature be 10-25 DEG C, condensation temperature is lower, more
Be conducive to chlorination mercuryvapour to be changed into solid and separate out recovery, when temperature is higher than 25 DEG C, the mercuric chloride response rate is low, and it is at room temperature
Slow distillation；When temperature is less than 10 DEG C, energy consumption increases.
As a further improvement on the present invention, step（4）Described in alkali be metal hydroxidess, metal carbonate or metal
Bicarbonate, for the hydrogen chloride adsorbed in neutralization activity charcoal；The metal carbonate is preferably sodium carbonate, potassium carbonate, described
Alkali metal bicarbonate salt is preferably sodium bicarbonate, potassium bicarbonate, and the metal hydroxidess are preferably sodium hydroxide, potassium hydroxide,
More preferably mass fraction for 20-54% sodium hydrate aqueous solution, excessive concentration, when reaching hypersaturated state, part hydroxide
Sodium granule separates out the micro channel that can be blocked in activated carbon；Sodium hydrate aqueous solution volume is larger when concentration is too low, and it is right to increased
The requirement of equipment volume or batch operation increased process time.
Compared with prior art, give up in generated by polyvinyl chloride by calcium carbide of the invention production mercury catalyst recovery method have with
Lower advantage：Heating-up temperature is low when reclaiming mercuric chloride, it is only necessary to carry out at 90-120 DEG C, and the response rate is up to 95%, high purity
99.5%；After treatment purity is high for the activated carbon of recovery, and the response rate is up to 92%, recovers adsorption activity, and micro pore surface area is recovered
To 1000-1200m2/ g, void content returns to 0.3-0.6ml/g；In addition this method is simple to operate, energy consumption is reduced, green ring
Protect pollution-free, moreover it is possible to effectively remove organic substance and the hydrochloric acid materials such as vinyl chloride.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further, it should be appreciated that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention；In addition, it is to be understood that after present disclosure has been read, those skilled in the art can
To make various changes or modifications to the present invention, these equivalent form of values also fall within appended claims limited range.
Embodiment 1：
The recovery method of useless mercury catalyst, comprises the steps in a kind of generated by polyvinyl chloride by calcium carbide production：
（1）The useless mercury catalysts of first 100g are crushed to fineness for 40 mesh, and the useless hydrargyrum catalysis system refers to and be adsorbed with activated carbon 2% chlorination
The decaying catalyst of hydrargyrum, 1% hydrogen chloride and 0.4% vinyl chloride；
（2）Useless mercury catalyst after by above-mentioned crushing removes vinyl chloride with 150ml extraction with carbon disulfide, is filtrated to get filtering residue；
（3）Above-mentioned filtering residue is heated to into 90 DEG C under the conditions of lucifuge, distillation 120min obtains chlorination mercuryvapour, then at 18 DEG C
Condensation is reclaimed and obtains the mercuric chloride solid that 1.92g purity is 99.5%, and the response rate is 96%；
（4）Remaining filtering residue after above-mentioned recovery mercuric chloride is processed with the sodium hydrate aqueous solution that 120g mass fractions are 20%, mistake
Filter, is dried at 80 DEG C, and recovery obtains 88.9g activated carbons, and the response rate is 92%, and its micro pore surface area returns to 1000m2/ g, hole
Gap volume returns to 0.3ml/g.
Embodiment 2：
The recovery method of useless mercury catalyst, comprises the steps in a kind of generated by polyvinyl chloride by calcium carbide production：
（1）The useless mercury catalysts of first 100g are crushed to fineness for 80 mesh, and the useless hydrargyrum catalysis system refers to and be adsorbed with activated carbon 3.8% chlorine
Change the decaying catalyst of hydrargyrum, 0.5% hydrogen chloride and 0.1% vinyl chloride；
（2）Useless mercury catalyst after by above-mentioned crushing removes vinyl chloride with 300ml extraction with carbon disulfide, is filtrated to get filtering residue；
（3）Above-mentioned filtering residue is heated to into 120 DEG C under the conditions of lucifuge, distillation 30min obtains chlorination mercuryvapour, then at 10 DEG C
Condensation is reclaimed and obtains the mercuric chloride solid that 3.69g purity is 99.6%, and the response rate is 97%；
（4）Remaining filtering residue after above-mentioned recovery mercuric chloride is processed with the sodium hydrate aqueous solution that 80g mass fractions are 54%, mistake
Filter, is dried at 80 DEG C, and recovery obtains 88.9g activated carbons, and the response rate is 93%, and its micro pore surface area returns to 1200m2/ g, hole
Gap volume returns to 0.6ml/g.
Embodiment 3：
The recovery method of useless mercury catalyst, comprises the steps in a kind of generated by polyvinyl chloride by calcium carbide production：
（1）The useless mercury catalysts of first 100g are crushed to fineness for 60 mesh, and the useless hydrargyrum catalysis system refers to and be adsorbed with activated carbon 2.9% chlorine
Change the decaying catalyst of hydrargyrum, 0.7% hydrogen chloride and 0.2% vinyl chloride；
（2）Useless mercury catalyst after by above-mentioned crushing removes vinyl chloride with 220ml extraction with carbon disulfide, is filtrated to get filtering residue；
（3）Above-mentioned filtering residue is heated to into 105 DEG C under the conditions of lucifuge, distillation 75min obtains chlorination mercuryvapour, then at 25 DEG C
Condensation is reclaimed and obtains the mercuric chloride solid that 2.76g purity is 99.5%, and the response rate is 95%；
（4）Remaining filtering residue after above-mentioned recovery mercuric chloride is processed with the sodium hydrate aqueous solution that 105g mass fractions are 35%, mistake
Filter, is dried at 80 DEG C, and recovery obtains 88.5g activated carbons, and the response rate is 92%, and its micro pore surface area returns to 1108m2/ g, hole
Gap volume returns to 0.46ml/g.
Claims (10)
1. the recovery method of useless mercury catalyst during a kind of generated by polyvinyl chloride by calcium carbide is produced, it is characterised in that comprise the steps：
（1）First useless mercury catalyst is crushed to into certain fineness, the useless hydrargyrum catalysis system refers to and be adsorbed with activated carbon mercuric chloride, chlorination
The decaying catalyst of hydrogen and vinyl chloride；
（2）Useless mercury catalyst after by above-mentioned crushing removes vinyl chloride with extraction with carbon disulfide, is filtrated to get filtering residue；
（3）Above-mentioned filtering residue is heated under the conditions of lucifuge and obtains chlorination mercuryvapour, mercuric chloride solid is reclaimed in then condensation；
（4）By remaining filtering residue alkali process after above-mentioned recovery mercuric chloride, the hydrogen chloride of absorption is neutralized, filtered, be dried, reclaimed and live
Property charcoal.
2. give up the recovery method of mercury catalyst in a kind of generated by polyvinyl chloride by calcium carbide production according to claim 1, its feature
It is：Step（1）Described in give up and be respectively the hydrogen chloride of the mercuric chloride of 2-3.8%, 0.5-1% in mercury catalyst containing mass fraction
With the vinyl chloride of 0.1-0.4%.
3. give up the recovery method of mercury catalyst in a kind of generated by polyvinyl chloride by calcium carbide production according to claim 1, its feature
It is：Step（1）Described in give up mercury catalyst crush after fineness be 40-80 mesh.
4. give up the recovery method of mercury catalyst in a kind of generated by polyvinyl chloride by calcium carbide production according to claim 3, its feature
It is：Step（1）Described in give up mercury catalyst crush after fineness be 60 mesh.
5. give up the recovery method of mercury catalyst in a kind of generated by polyvinyl chloride by calcium carbide production according to claim 1, its feature
It is：Step（2）Described in give up mercury catalyst and Carbon bisulfide mass volume ratio be 1：1.5-3.
6. give up the recovery method of mercury catalyst in a kind of generated by polyvinyl chloride by calcium carbide production according to claim 5, its feature
It is：Step（2）Described in give up mercury catalyst and Carbon bisulfide mass volume ratio be 1：2.2.
7. give up the recovery method of mercury catalyst in a kind of generated by polyvinyl chloride by calcium carbide production according to claim 1, its feature
It is：Step（3）Described in heating-up temperature be 90-120 DEG C, heat time heating time is 30min-120min.
8. give up the recovery method of mercury catalyst in a kind of generated by polyvinyl chloride by calcium carbide production according to claim 1, its feature
It is：Step（3）Described in condensation temperature be 10-25 DEG C.
9. give up the recovery method of mercury catalyst in a kind of generated by polyvinyl chloride by calcium carbide production according to claim 1, its feature
It is：Step（4）Described in alkali be metal hydroxidess, metal carbonate or alkali metal bicarbonate salt.
10. give up the recovery method of mercury catalyst in a kind of generated by polyvinyl chloride by calcium carbide production according to claim 9, its feature
It is：The metal hydroxidess are the sodium hydrate aqueous solution that mass fraction is 20-54%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109097583A (en) * | 2018-08-22 | 2018-12-28 | 昆明理工大学 | A kind of method that clean and effective recycles useless low mercury catalyst |
| CN114229843A (en) * | 2021-12-24 | 2022-03-25 | 贵州重力科技环保有限公司 | Method for activating and regenerating waste activated carbon after harmless treatment of waste mercury catalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109097583A (en) * | 2018-08-22 | 2018-12-28 | 昆明理工大学 | A kind of method that clean and effective recycles useless low mercury catalyst |
| CN114229843A (en) * | 2021-12-24 | 2022-03-25 | 贵州重力科技环保有限公司 | Method for activating and regenerating waste activated carbon after harmless treatment of waste mercury catalyst |
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