CN111218148B - Method for producing putty powder by using industrial alkali residue white mud - Google Patents
Method for producing putty powder by using industrial alkali residue white mud Download PDFInfo
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- CN111218148B CN111218148B CN202010163222.0A CN202010163222A CN111218148B CN 111218148 B CN111218148 B CN 111218148B CN 202010163222 A CN202010163222 A CN 202010163222A CN 111218148 B CN111218148 B CN 111218148B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/34—Filling pastes
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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
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- 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
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention discloses a method for producing putty powder by using industrial alkali residue white mud, which comprises the following steps: s1: firstly, introducing alkali residue white mud into an autoclave for supercritical treatment; s2: introducing the materials in the kettle into a first purifying tank, adding a flocculating agent, fully stirring, standing for separation, and collecting filtrate and filter residues to obtain a filtrate; s3: adding water with the weight 3-4 times that of the filter residue in the step S2, adding a dispersing agent and a chelating agent, pulping, crushing, adding other raw materials of putty powder, and fully and uniformly stirring to obtain the putty powder. The putty powder prepared by the method disclosed by the invention is uniform in state in a container, free of caking, smooth in construction blade coating, excellent in whiteness, texture, grindability and water resistance, and good in bonding strength.
Description
Technical Field
The invention belongs to the field of alkali residue white mud treatment, and particularly relates to a method for producing putty powder by using industrial alkali residue white mud.
Background
The sodium carbonate is used as an important basic chemical raw material, is widely applied to industries such as metallurgy, chemical industry, building materials, papermaking, medicines, foods and the like, and generates a large amount of white sediment of alkali residue and white mud in the process of producing the sodium carbonate by an ammonia-soda process. Because of the large production amount and fine granularity of the alkaline residue white mud, the alkaline residue white mud has colloid property, slow sedimentation speed in water, high sediment water content, high dehydration difficulty and CaCO as the main component 3 、CaSO 4 CaO and Ca (OH) 2 CaCl (CaCl) 4 And NaCl, the chloride ion content is up to more than 15% in the absolute dry state, and the existence of a large amount of chloride ions causes great difficulty in the industrial utilization of the alkaline residue white mud. In the prior art, a large amount of alkaline residue white mud is disposed in a natural stacking, landfill or sea discharging mode, wherein the natural stacking or landfill occupies a large piece of land and causes environmental pollution to soil and a groundwater system; further sea displacement will have adverse effects on marine life and marine environment.
Putty (mud filling) is a decorative material for leveling the surface of a wall body, is a thick slurry paint, and is an indispensable product before painting the paint. Is applied to the primer or directly applied to the object to remove the defect of uneven surface of the coated object. The putty is divided into an inner wall and an outer wall, and the outer wall putty has high gumminess, high strength and low environmental protection index because of resisting wind, blowing and sun. The putty for the inner wall has good comprehensive index, is healthy and environment-friendly, so that the putty for the inner wall is not used externally and the putty for the outer wall is not used internally. Typically the putty is gypsum or cement based so that the surface roughness is relatively easy to bond firmly.
The alkaline residue white mud contains rich calcium salt, so that the calcium carbonate is extracted from the alkaline residue white mud to produce putty powder, and the alkaline residue white mud is provided with another treatment mode, so that the alkaline residue white mud has good market prospect.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a method for producing putty powder by using industrial alkaline residue white mud, which has the advantages of effectively removing elements such as chloride ions, sodium ions and the like in the alkaline residue white mud, improving the purity of the produced calcium carbonate and adding other auxiliary materials to prepare the putty powder.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for producing putty powder by using industrial alkali residue white mud comprises the following steps:
s1: firstly, introducing alkaline residue white mud into an autoclave, carrying out heat preservation and stirring for 2-3 hours at the temperature of 32-35 ℃ in a first supercritical state, then introducing carbon dioxide, maintaining the pressure in the autoclave at 7.5-7.8MPa, and maintaining the pressure for 2-3 hours;
in a second supercritical state, preserving heat and stirring for 1h at 40-45 ℃, then introducing carbon dioxide, maintaining the pressure in the kettle at 8-10MPa, and maintaining the pressure for 1-2h;
in a third supercritical state, preserving heat and stirring for 1h at 45-50 ℃, then introducing carbon dioxide, maintaining the pressure in the kettle at 10-11MPa, and maintaining the pressure for 0.5-1h;
s2: introducing the materials in the kettle into a first purifying tank, adding a flocculating agent, fully stirring, standing for separation, and collecting filtrate and filter residues to obtain a filtrate;
s3: adding water with the weight 3-4 times that of the filter residue in the step S2, adding a dispersing agent and a chelating agent, heating to 50-60 ℃, preserving heat, and filtering; pulping with water 0.5-1 times of the weight of the filter residue, filtering, and repeating pulping operation for 3-5 times to obtain fully pulped filter residue;
s4: fully pulping filter residues, and drying to obtain powder;
s5: and then adding glue, cellulose, wetting agent, thickener and white cement after micro-crushing the powder, and fully and uniformly mixing to obtain the putty powder.
By adopting the technical scheme, under the three supercritical states, supercritical temperature and pressure are gradually increased, under the continuous action of critical carbon dioxide, dissolved calcium ions are absorbed by the carbon dioxide in a fluid state, chemical equilibrium is enabled to move towards the direction of generating calcium carbonate precipitate, calcium carbonate is continuously generated, then filter residues containing the calcium carbonate are obtained through flocculating agent, sedimentation and filtration, and then the filter residues are subjected to dispersing, chelating and pulping treatment, so that the calcium carbonate powder with higher purity is obtained. And (3) mixing the calcium carbonate powder with glue, cellulose, a wetting agent, a thickening agent and white cement to obtain putty powder.
Carbon dioxide, at a temperature higher than the critical temperature tc= 31.26 ℃ and a pressure higher than the critical pressure pc=72.9 atm, undergoes a change in properties, its density being close to liquid, its viscosity being close to gas, and its diffusion coefficient being 100 times that of liquid, and thus has a surprising capacity for dissolution, with which various substances can be dissolved.
The invention is further provided with: and (3) flocculating agent polyacrylamide in the step S2.
The invention is further provided with: and the heat preservation time in the step S3 is 2-3h.
The invention is further provided with: the temperature during pulping in the step S3 is 40-45 ℃.
The invention is further provided with: the dispersing agent in the step S3 is ethylene diamine tetraacetic acid disodium salt
The invention is further provided with: the chelating agent in the step S3 is an amino acid chelating agent.
By adopting the technical scheme, the technological parameters of each operation in the steps S2 and S3 are defined, and flocculating agents are added to guide the calcium carbonate to flocculate and settle; meanwhile, the filter residues are well dispersed through the dispersing agent, the filter residues are convenient to filter, the amino acid chelating agent is added to be matched with the dispersing agent, the agglomeration of fine particles is reduced to the greatest extent, the activated calcium carbonate powder with high dispersion and low free alkali content is obtained, the subsequent filtering and crushing are convenient, and meanwhile, the beating is carried out, so that Cl, na and other elements in the filter residues can be dissolved into the filtrate to be removed;
the invention is further provided with: in the step S5, the powder, glue, cellulose, wetting agent, thickener and white cement are added according to the weight proportion: glue: cellulose: wetting agent: and (3) a thickening agent: white cement=10:20-30:2-5:1-2:1-2:50-60.
The invention is further provided with: the thickener in the step S5 is methyl cellulose ether.
The invention is further provided with: the wetting agent in the step S5 is span-80.
By adopting the technical scheme, in the step S5, the putty powder is obtained after the proper putty powder raw materials are fully stirred and mixed, and the wetting agent can enable water to spread on the surface of the solid material or penetrate into the surface of the solid material by reducing the surface tension or interfacial tension of the putty powder raw materials, so that the solid material is moistened; the thickener can increase the surface tension of white cement and calcium carbonate powder, and can enable the white cement and the calcium carbonate powder to be better coated on a wall body.
In summary, the invention has the following advantages:
1. according to the preparation method, after calcium carbonate is extracted and recovered from industrial alkaline residue white mud, glue, cellulose, a wetting agent, a thickening agent and white cement are added to form putty powder, and the putty powder has high bonding strength.
2. According to the preparation method, the industrial direct-discharge alkaline residue white mud is treated under the critical condition of carbon dioxide, so that the soluble calcium in the alkaline residue white mud can be well converted into insoluble calcium carbonate to be separated out, and the method is changed into Cheng Modu harmless, is simple to operate and is convenient for industrial production.
Detailed Description
The following description of the present invention will be made clearly and fully, and it is apparent that the embodiments described are some, but not all, of the embodiments of the present invention.
Example 1
A method for producing putty powder by using industrial alkali residue white mud comprises the following steps:
s1: firstly, introducing alkaline residue white mud into an autoclave, carrying out heat preservation and stirring for 2 hours at the temperature of 32 ℃ in a first supercritical state, then introducing carbon dioxide, maintaining the pressure in the autoclave at 7.5-7.8MPa, and maintaining the pressure for 2 hours;
in a second supercritical state, preserving heat and stirring for 1h at 40 ℃, then introducing carbon dioxide, maintaining the pressure in the kettle at 8-10MPa, and maintaining the pressure for 1h;
in a third supercritical state, preserving heat and stirring for 1h at 45 ℃, then introducing carbon dioxide, maintaining the pressure in the kettle at 10-11MPa, and maintaining the pressure for 0.5h;
s2: introducing the materials in the kettle into a first purifying tank, adding polyacrylamide, fully stirring, standing for separation, and collecting filtrate and filter residues;
s3: adding water with the weight 3 times that of the filter residue into the filter residue obtained in the step S2, adding a dispersing agent and a chelating agent, heating to 50 ℃, preserving heat for 2 hours, and filtering; pulping with water with weight 0.5 times that of the filter residue, filtering, and repeating pulping operation for 3 times to obtain fully pulped filter residue; wherein the temperature in the pulping process is 40 ℃, the dispersing agent is disodium ethylenediamine tetraacetate, and the chelating agent is an amino acid chelating agent;
s4: fully pulping filter residues, and drying to obtain powder;
s5: and then adding glue, cellulose, span-80, methyl cellulose ether and white cement after carrying out micro-pulverization on the powder, and fully and uniformly mixing to obtain the putty powder. Wherein, the powder, glue, cellulose, span-80, methyl cellulose ether, white cement are added according to the weight proportion: glue: cellulose: span-80: methyl cellulose ether: white cement=10:20:2:1:1:50.
Example 2
A method for producing putty powder by using industrial alkali residue white mud comprises the following steps:
s1: firstly, introducing alkaline residue white mud into an autoclave, keeping the temperature and stirring for 2.5 hours at the temperature of 33 ℃ in a first supercritical state, then introducing carbon dioxide, maintaining the pressure in the autoclave at 7.5-7.8MPa, and maintaining the pressure for 2.5 hours;
in a second supercritical state, preserving heat and stirring for 1h at 43 ℃, then introducing carbon dioxide, maintaining the pressure in the kettle at 8-10MPa, and maintaining the pressure for 1.5h;
in a third supercritical state, preserving heat and stirring for 1h at 47 ℃, then introducing carbon dioxide, maintaining the pressure in the kettle at 10-11MPa, and maintaining the pressure for 0.7h;
s2: introducing the materials in the kettle into a first purifying tank, adding polyacrylamide, fully stirring, standing for separation, and collecting filtrate and filter residues;
s3: adding water with the weight 3.5 times that of the filter residue in the step S2, adding a dispersing agent and a chelating agent, heating to 55 ℃, preserving heat for 2.5 hours, and filtering; pulping with water with weight 0.7 times of that of the filter residue, filtering, and repeating pulping operation for 4 times to obtain fully pulped filter residue; wherein the temperature in the pulping process is 43 ℃, the dispersing agent is disodium ethylenediamine tetraacetate, and the chelating agent is an amino acid chelating agent;
s4: fully pulping filter residues, and drying to obtain powder;
s5: and then adding glue, cellulose, span-80, methyl cellulose ether and white cement after carrying out micro-pulverization on the powder, and fully and uniformly mixing to obtain the putty powder. Wherein, the powder, glue, cellulose, span-80, methyl cellulose ether, white cement are added according to the weight proportion: glue: cellulose: span-80: methyl cellulose ether: white cement=10:25:3:1.5:1.5:55.
Example 3
A method for producing putty powder by using industrial alkali residue white mud comprises the following steps:
s1: firstly, introducing alkaline residue white mud into an autoclave, preserving heat and stirring for 3 hours at the first supercritical state at 35 ℃, then introducing carbon dioxide, maintaining the pressure in the autoclave at 7.5-7.8MPa, and maintaining the pressure for 3 hours;
in a second supercritical state, preserving heat and stirring for 1h at 45 ℃, then introducing carbon dioxide, maintaining the pressure in the kettle at 8-10MPa, and maintaining the pressure for 2h;
in a third supercritical state, preserving heat and stirring for 1h at 50 ℃, then introducing carbon dioxide, maintaining the pressure in the kettle at 10-11MPa, and maintaining the pressure for 1h;
s2: introducing the materials in the kettle into a first purifying tank, adding polyacrylamide, fully stirring, standing for separation, and collecting filtrate and filter residues;
s3: adding water with the weight 4 times that of the filter residue into the filter residue obtained in the step S2, adding a dispersing agent and a chelating agent, heating to 60 ℃, preserving heat for 3 hours, and filtering; pulping with 1 time of water, filtering, and repeating pulping operation for 5 times to obtain fully pulped residue; wherein the temperature in the pulping process is 45 ℃, the dispersing agent is disodium ethylenediamine tetraacetate, and the chelating agent is an amino acid chelating agent;
s4: fully pulping filter residues, and drying to obtain powder;
s5: and then adding glue, cellulose, span-80, methyl cellulose ether and white cement after carrying out micro-pulverization on the powder, and fully and uniformly mixing to obtain the putty powder. Wherein, the powder, glue, cellulose, span-80, methyl cellulose ether, white cement are added according to the weight proportion: glue: cellulose: span-80: methyl cellulose ether: white cement=10:30:5:2:2:60.
Comparative example 1
Step S1 is omitted, and the rest conditions are consistent;
comparative example 2
Step S2 is not carried out, and the other conditions are consistent;
the addition amounts of the flocculating agent, the dispersing agent and the chelating agent in the examples 1-3 and the comparative examples 1-2 are respectively 0.02%, 0.005% and 0.001% of the weight of the alkaline residue white mud; micronizing to 200-300 mesh sieve. The filtering is preferably plate frame pressure filtering;
the putty powder prepared in examples 1-3 and comparative examples 1-2 was tested according to JG/T298-2010 and other requirements, and the test results are shown in the following table:
as can be seen from the above table, the putty powder prepared in examples 1 to 3 was uniform in state in a container without caking, smooth in application blade coating, excellent in whiteness, texture, grindability and water resistance, and also had a good adhesive strength of 1.25 to 1.37MPa, whereas the putty powder prepared in comparative examples 1 and 2 again was inferior in state in a container, workability, whiteness, texture, grindability and water resistance, and also had a low adhesive strength, because it was not possible to remove impurities (such as chloride ions, sodium ions, etc.) in the filter residue well.
The above embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalent substitutions, improvements, etc. within the design concept of the present invention should be included in the scope of the present invention.
Claims (3)
1. The method for producing the putty powder by using the industrial alkali residue white mud is characterized by comprising the following steps of:
s1: firstly, introducing alkaline residue white mud into an autoclave, carrying out heat preservation and stirring for 2-3 hours at the temperature of 32-35 ℃ in a first supercritical state, then introducing carbon dioxide, maintaining the pressure in the autoclave at 7.5-7.8MPa, and maintaining the pressure for 2-3 hours;
in a second supercritical state, preserving heat and stirring for 1h at 40-45 ℃, then introducing carbon dioxide, maintaining the pressure in the kettle at 8-10MPa, and maintaining the pressure for 1-2h;
in a third supercritical state, preserving heat and stirring for 1h at 45-50 ℃, then introducing carbon dioxide, maintaining the pressure in the kettle at 10-11MPa, and maintaining the pressure for 0.5-1h;
s2: introducing the materials in the kettle into a first purifying tank, adding a flocculating agent, fully stirring, standing for separation, and collecting filtrate and filter residues to obtain a filtrate;
s3: adding water with the weight 3-4 times that of the filter residue in the step S2, adding a dispersing agent and a chelating agent, heating to 50-60 ℃, preserving heat, and filtering; pulping with water 0.5-1 times of the weight of the filter residue, filtering, and repeating pulping operation for 3-5 times to obtain fully pulped filter residue;
s4: fully pulping filter residues, and drying to obtain powder;
s5: then adding glue, cellulose, wetting agent, thickener and white cement after micro-crushing the powder, and obtaining the putty powder after fully and uniformly mixing;
wherein, the flocculant in the step S2 is polyacrylamide;
the dispersing agent in the step S3 is ethylene diamine tetraacetic acid disodium salt;
the chelating agent in the step S3 is an amino acid chelating agent;
the thickener in the step S5 is methyl cellulose ether;
the wetting agent in the step S5 is span-80;
in the step S5, the powder, glue, cellulose, wetting agent, thickener and white cement are added according to the weight proportion: glue: cellulose: wetting agent: and (3) a thickening agent: white cement=10:20-30:2-5:1-2:1-2:50-60.
2. The method for producing putty powder by using industrial alkali residue white mud as set forth in claim 1, wherein the heat preservation time in step S3 is 2-3h.
3. The method for producing putty powder by using industrial alkaline residue white mud as set forth in claim 1, wherein the temperature at the time of beating in step S3 is 40-45 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591029A (en) * | 2008-05-28 | 2009-12-02 | 北京紫光英力化工技术有限公司 | Causticizing process prepares the novel process of caustic soda and super fine calcium carbonate |
| CN106497209A (en) * | 2016-12-28 | 2017-03-15 | 芜湖普乐士新型建筑材料配套有限公司 | A kind of putty powder for exterior wall |
| CN107722708A (en) * | 2017-11-29 | 2018-02-23 | 广州市龙芝圆科技有限公司 | A kind of environmental friendly putty powder |
| CN110092625A (en) * | 2019-05-24 | 2019-08-06 | 华南理工大学 | A kind of cement mixed mortar preparing the preparation of calcium carbonate superfine powder powder with alkaline residue |
-
2020
- 2020-03-10 CN CN202010163222.0A patent/CN111218148B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591029A (en) * | 2008-05-28 | 2009-12-02 | 北京紫光英力化工技术有限公司 | Causticizing process prepares the novel process of caustic soda and super fine calcium carbonate |
| CN106497209A (en) * | 2016-12-28 | 2017-03-15 | 芜湖普乐士新型建筑材料配套有限公司 | A kind of putty powder for exterior wall |
| CN107722708A (en) * | 2017-11-29 | 2018-02-23 | 广州市龙芝圆科技有限公司 | A kind of environmental friendly putty powder |
| CN110092625A (en) * | 2019-05-24 | 2019-08-06 | 华南理工大学 | A kind of cement mixed mortar preparing the preparation of calcium carbonate superfine powder powder with alkaline residue |
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