CN108128783A - A kind of preparation method of 3A zeolite molecular sieves original powder - Google Patents
A kind of preparation method of 3A zeolite molecular sieves original powder Download PDFInfo
- Publication number
- CN108128783A CN108128783A CN201810215805.6A CN201810215805A CN108128783A CN 108128783 A CN108128783 A CN 108128783A CN 201810215805 A CN201810215805 A CN 201810215805A CN 108128783 A CN108128783 A CN 108128783A
- Authority
- CN
- China
- Prior art keywords
- zeolite molecular
- original powder
- molecular sieves
- preparation
- meta
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/14—Type A
- C01B39/16—Type A from aqueous solutions of an alkali metal aluminate and an alkali metal silicate excluding any other source of alumina or silica but seeds
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a kind of preparation methods of 3A zeolite molecular sieves original powder.The mixed solution of aluminium hydroxide potassium hydroxide and sodium hydroxide is dissolved, meta-aluminate solution is made, then pulp reaction is carried out with sodium silicate solution, heat up crystallization, separation, washing, drying can directly obtain exchange degree height, the good 3A zeolite molecular sieve original powder products of absorption property.Invention not only simplifies technological processes prepared by traditional 3A zeolite molecular sieves original powder, without carrying out secondary potassium exchange with 4A molecular screen primary powders, the manufacturing cost of 3A zeolite molecular sieve original powders is greatly reduced, production process environmental protection is without discharging of waste liquid, and products obtained therefrom exchange degree is high, it is easy to control, adsorption capacity is high, has broad application prospects in molecular sieve industry.
Description
Technical field
The present invention relates to zeolite preparing technical field, more particularly to a kind of preparation method of 3A zeolite molecular sieves original powder.
Background technology
3A molecular sieves are mainly used for adsorbing water, do not adsorb any molecule that diameter is more than 3A, the good 3A molecular sieves production of performance
Product have faster adsorption rate, more regeneration times, higher crushing strength and contamination resistance, improve molecular sieve
Utilization ratio and extend the service life of molecular sieve.3A molecular sieves are liquid phase depth drying, essence in oil, chemical industry
Preferred drier necessary to refining, polymerization.At present, the raw material 3A zeolite molecular sieve original powder 4A zeolites of 3A zeolite molecular sieves are all
Each enterprise is raw material with the 4A zeolite molecular sieve original powders after crystallization, washing, adds in certain according to requirement of the client to potassium exchange degree
The potassium chloride and water of amount, carry out ion exchange at a certain temperature, obtain 3A zeolite molecular sieve original powder products.It is handed over using ion
It changes method and prepares 3A zeolite molecular sieve original powders, although using the relatively low Potassium Chloride Product of price, the final utilization of potassium chloride
Rate only has insufficient half, while technological process is long, needs to be made as raw material with crystallization and the 4A zeolite molecular sieves original powder washed
The repetition and waste of Cheng Shui, steam and electricity, generally speaking cost is also higher.Meanwhile ion-exchange prepares 3A zeolite molecular sieves original
Powder, most fatal be exchange after mother liquor can not recycle, in mother liquor containing a large amount of sodium, potassium, rate ion, direct emission
Very big pollution can be caused to environment.
Increasingly serious with environmentally friendly form, every profession and trade is more and more stringenter to the emission request of " three wastes ".Traditional 3A boilings
Stone molecular screen primary powder manufacturing enterprise needs outer row due to there is a large amount of mother liquor that exchanges that can not reuse, thus is forced to stop production, and makes
Into the in short supply of 3A zeolite molecular sieve original powders.Although the enterprise that there is waste treatment capacity in part is still given birth to using conventional method
Production, but due to the imbalance between supply and demand in market, the price of product is also greatly improved.The anxiety of 3A Molecular sieve raw materials, direct shadow
Ring the product demand to the application, especially hollow glass industry in downstream.Even, occur many being replaced with 4A molecular sieves in the market
The phenomenon that for 3A zeolite products, directly influence the development of many application fields.Therefore, research one kind can reduce 3A zeolites
Molecular screen primary powder production cost, and can be completely without the preparation method of the 3A zeolite molecular sieve original powders of discharge of wastewater, to meet
The demand of growing 3A zeolite molecular sieve industries, is of great significance.
Invention content
The present invention provides a kind of preparation method of 3A zeolite molecular sieves original powder aiming at above-mentioned defect, this hair
The 3A zeolite molecular sieves original powder of preparation prepared by bright method has high exchange degree and adsorptivity, while can ensure 3A zeolites point again
Easy to operate, non-wastewater discharge in son sieve original powder product preparation process.
A kind of preparation method technical solution of 3A zeolite molecular sieves original powder of the present invention is, by aluminium hydroxide potassium hydroxide
It is dissolved with the mixed solution of sodium hydroxide, meta-aluminate solution is made, then pulp reaction is carried out with sodium silicate solution, then
Heating crystallization is carried out again, and separation, washing, drying can directly obtain exchange degree height, the good 3A zeolite molecular sieves of absorption property
Original powder product.
A kind of preparation method of 3A zeolite molecular sieves original powder.Processing step includes successively：
（1）Potassium hydroxide, sodium hydroxide and water are mixed, are prepared into aqueous slkali；
（2）Aluminium hydroxide is added to step（1）In the aqueous slkali, heat temperature raising is dissolved into meta-aluminate solution；
（3）By step（2）The meta-aluminate solution mixes after dilution with sodium silicate solution, carries out pulp reaction, then
Carry out heating crystallization；
（4）By step（3）Obtained crystallization liquid is filtered, washs, drying to get high, the good 3A of absorption property to exchange degree
Zeolite molecular sieve original powder product.
Step（1）In, K2O/Na2O molar ratios are 2-3, in the aqueous slkali after being diluted with water, K2O+Na2O's is a concentration of
200-300g/l。
Step（2）In, the addition of aluminium hydroxide is calculated according to the α k of the meta-aluminate solution of preparation in 2.1-2.5.
Step（3）In, meta-aluminate solution is diluted with water to Al2O3A concentration of 65-100g/l.
Step（3）In, the modulus of sodium silicate solution used is 3-3.5, SiO2A concentration of 100-200g/l.
Step（3）In, after meta-aluminate and sodium silicate solution mixing, the temperature of pulp is 30-80 DEG C, time 30-
60min, 90-98 DEG C of crystallization temperature, crystallization time 2-3h.
Step（4）In, obtained 3A zeolite molecular sieves original powder product, K2O content 13-14%, Static Water adsorb more than
25.5mg/g。。
Beneficial effects of the present invention are：The present invention overcomes existing 3A zeolites fractionated molecules to sieve in original powder preparation process, largely
Discharging of waste liquid containing chlorine and the shortcomings that have to pass through secondary exchange.The method of the present invention was produced in 3A zeolite molecular sieve original powders
Cheng Zhong dissolves aluminium hydroxide with sodium hydroxide and potassium hydroxide, and the meta-aluminate of preparation has guarantor as silicon source, not only product quality
Card, and does not have discharging of waste liquid in preparation process, easy to operate there are no need to carry out secondary exchange with 4A zeolites, reduces production
Cost will bring profound significance to the development of molecular sieve absorption industry.
Specific embodiment：
For a better understanding of the present invention, below with specific example come the technical solution that the present invention will be described in detail, but it is of the invention
It is not limited thereto.
Embodiment 1
(1) by potassium hydroxide and sodium hydroxide according to K2O/Na2The molar ratio 2.6 of O mixes, and adds distillation water dissolution, is configured to K2O
+Na2The aqueous slkali of a concentration of 280g/l of O.
（2）With a certain amount of aluminium hydroxide, according to α after dissolvingk2.2, it adds in above-mentioned aqueous slkali, dissolves by heating, be used in combination
Distilled water is diluted to Al2O3The meta-aluminate solution of a concentration of 75g/l.
（3）By modulus 3.1, SiO2The water glass solution of a concentration of 120g/l and above-mentioned meta-aluminate, according to SiO2/
Al2O3Molar ratio 2.0 mix, the pulp 30min under the conditions of 45 DEG C, then body temperature is to 95 DEG C, carries out crystallization.
（4）To get to the slurry of qualified 3A zeolite molecular sieve original powders after crystallization 2h.
（5）3A zeolites slurry is filtered, washed, is dried to get to 3A zeolite molecular sieve original powder products, K2O content
It is 13.6%, Static Water is adsorbed as 26.2mg/g.
Embodiment 2
（1）By potassium hydroxide and sodium hydroxide according to K2O/Na2The molar ratio 2.1 of O mixes, and adds distillation water dissolution, is configured to K2O+
Na2The aqueous slkali of a concentration of 260g/l of O.
（2）With a certain amount of aluminium hydroxide, according to α after dissolvingk2.1, it adds in above-mentioned aqueous slkali, dissolves by heating, be used in combination
Distilled water is diluted to Al2O3The meta-aluminate solution of a concentration of 75g/l.
（3）By modulus 3.1, SiO2The water glass solution of a concentration of 120g/l and above-mentioned meta-aluminate, according to SiO2/
Al2O3Molar ratio 2.0 mix, the pulp 45min under the conditions of 52 DEG C, then body temperature is to 90 DEG C, carries out crystallization.
（4）To get to the slurry of qualified 3A zeolite molecular sieve original powders after crystallization 2.5h.
（5）3A zeolites slurry is filtered, washed, is dried to get to 3A zeolite molecular sieve original powder products, K2O content
It is 13.1%, Static Water is adsorbed as 26.4mg/g.
Embodiment 3
（1）By potassium hydroxide and sodium hydroxide according to K2O/Na2The molar ratio 2.1 of O mixes, and adds distillation water dissolution, is configured to K2O+
Na2The aqueous slkali of a concentration of 260g/l of O.
（2）With a certain amount of aluminium hydroxide, according to α after dissolvingk2.1, it adds in above-mentioned aqueous slkali, dissolves by heating, be used in combination
Distilled water is diluted to Al2O3The meta-aluminate solution of a concentration of 85g/l.
（3）By modulus 3.1, SiO2The water glass solution of a concentration of 106g/l and above-mentioned meta-aluminate, according to SiO2/
Al2O3Molar ratio 2.0 mix, the pulp 45min under the conditions of 65 DEG C, then body temperature is to 96 DEG C, carries out crystallization.
（4）To get to the slurry of qualified 3A zeolite molecular sieve original powders after crystallization 2h.
（5）3A zeolites slurry is filtered, washed, is dried to get to 3A zeolite molecular sieve original powder products, K2O content
It is 13.2%, Static Water is adsorbed as 26.1mg/g.
Embodiment 4
（1）By potassium hydroxide and sodium hydroxide according to K2O/Na2The molar ratio 2.3 of O mixes, and adds distillation water dissolution, is configured to K2O+
Na2The aqueous slkali of a concentration of 240g/l of O.
（2）It with a certain amount of aluminium hydroxide, according to α k2.4 after dissolving, adds in above-mentioned aqueous slkali, dissolves by heating, be used in combination
Distilled water is diluted to Al2O3The meta-aluminate solution of a concentration of 62g/l.
（3）By modulus 3.0, SiO2The water glass solution of a concentration of 145g/l and above-mentioned meta-aluminate, according to SiO2/
Al2O3Molar ratio 2.0 mix, the pulp 45min under the conditions of 56 DEG C, then body temperature is to 95 DEG C, carries out crystallization.
（4）To get to the slurry of qualified 3A zeolite molecular sieve original powders after crystallization 2.5h.
（5）3A zeolites slurry is filtered, washed, is dried to get to 3A zeolite molecular sieve original powder products, K2O content
It is 13.3%, Static Water is adsorbed as 25.9mg/g.
Embodiment 5
（1）By potassium hydroxide and sodium hydroxide according to K2O/Na2The molar ratio 2.9 of O mixes, and adds distillation water dissolution, is configured to K2O+
Na2The aqueous slkali of a concentration of 230g/l of O.
（2）With a certain amount of aluminium hydroxide, according to α after dissolvingk2.3, it adds in above-mentioned aqueous slkali, dissolves by heating, be used in combination
Distilled water is diluted to Al2O3The meta-aluminate solution of a concentration of 78g/l.
（3）By modulus 3.1, SiO2The water glass solution of a concentration of 102g/l and above-mentioned meta-aluminate, according to SiO2/
Al2O3Molar ratio 2.0 mix, the pulp 35min under the conditions of 55 DEG C, then body temperature is to 94 DEG C, carries out crystallization.
（4）To get to the slurry of qualified 3A zeolite molecular sieve original powders after crystallization 2h.
（5）3A zeolites slurry is filtered, washed, is dried to get to 3A zeolite molecular sieve original powder products, K2O content
It is 13.7%, Static Water is adsorbed as 25.8mg/g.
Claims (8)
1. a kind of preparation method of 3A zeolite molecular sieves original powder, which is characterized in that by aluminium hydroxide potassium hydroxide and hydroxide
The mixed solution of sodium is dissolved, and meta-aluminate solution is made, then carry out pulp reaction with sodium silicate solution, is then risen again
Warm crystallization, separation, washing, drying can directly obtain exchange degree height, the good 3A zeolite molecular sieve original powder products of absorption property.
2. a kind of preparation method of 3A zeolite molecular sieves original powder according to claim 1, which is characterized in that processing step according to
It is secondary including：
（1）Potassium hydroxide, sodium hydroxide and water are mixed, are prepared into aqueous slkali；
（2）Aluminium hydroxide is added to step（1）In the aqueous slkali, heat temperature raising is dissolved into meta-aluminate solution；
（3）By step（2）The meta-aluminate solution mixes after dilution with sodium silicate solution, carries out pulp reaction, then
Carry out heating crystallization；
（4）By step（3）Obtained crystallization liquid is filtered, washs, drying to get high, the good 3A of absorption property to exchange degree
Zeolite molecular sieve original powder product.
A kind of 3. preparation method of 3A zeolite molecular sieves original powder according to claim 2, which is characterized in that step（1）In,
KO/Na2O molar ratios are 2-3, in the aqueous slkali after being diluted with water, K2O+Na2A concentration of 200-300g/l of O.
A kind of 4. preparation method of 3A zeolite molecular sieves original powder according to claim 2, which is characterized in that step（2）In,
The addition of aluminium hydroxide is calculated according to the α k of the meta-aluminate solution of preparation in 2.1-2.5.
A kind of 5. preparation method of 3A zeolite molecular sieves original powder according to claim 2, which is characterized in that step（3）In,
Meta-aluminate solution is diluted with water to Al2O3A concentration of 65-100g/l.
A kind of 6. preparation method of 3A zeolite molecular sieves original powder according to claim 2, which is characterized in that step（3）In,
The modulus of sodium silicate solution used is 3-3.5, SiO2A concentration of 100-200g/l.
A kind of 7. preparation method of 3A zeolite molecular sieves original powder according to claim 2, which is characterized in that step（3）In,
After meta-aluminate and sodium silicate solution mixing, the temperature of pulp is 30-80 DEG C, time 30-60min, 90-98 DEG C of crystallization temperature,
Crystallization time 2-3h.
A kind of 8. preparation method of 3A zeolite molecular sieves original powder according to claim 1, which is characterized in that step（4）In,
Obtained 3A zeolite molecular sieves original powder product, K2O content 13-14%, Static Water adsorb more than 25.5mg/g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810215805.6A CN108128783B (en) | 2018-03-15 | 2018-03-15 | Preparation method of 3A zeolite molecular sieve raw powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810215805.6A CN108128783B (en) | 2018-03-15 | 2018-03-15 | Preparation method of 3A zeolite molecular sieve raw powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108128783A true CN108128783A (en) | 2018-06-08 |
| CN108128783B CN108128783B (en) | 2021-04-09 |
Family
ID=62431278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810215805.6A Active CN108128783B (en) | 2018-03-15 | 2018-03-15 | Preparation method of 3A zeolite molecular sieve raw powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108128783B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU112503U1 (en) * | 2011-08-29 | 2012-01-10 | Открытое акционерное общество "Научно-производственное предприятие "Контакт" | WIDE KLISTRON |
| CN106892438A (en) * | 2017-02-10 | 2017-06-27 | 山东鲁北企业集团总公司 | A kind of preparation method of 4A zeolites |
-
2018
- 2018-03-15 CN CN201810215805.6A patent/CN108128783B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU112503U1 (en) * | 2011-08-29 | 2012-01-10 | Открытое акционерное общество "Научно-производственное предприятие "Контакт" | WIDE KLISTRON |
| CN106892438A (en) * | 2017-02-10 | 2017-06-27 | 山东鲁北企业集团总公司 | A kind of preparation method of 4A zeolites |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108128783B (en) | 2021-04-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101569852B (en) | Method for modifying natural zeolite powder | |
| CN107640777A (en) | A kind of method for preparing big/mesoporous zeolite molecular sieve of crystal seed induction | |
| CN103964462B (en) | The method of microwave solid source Fast back-projection algorithm zeolite molecular sieve | |
| CN104291349A (en) | Method for preparing P type molecular sieve by using coal ash as raw material | |
| CN106984266A (en) | A kind of method that VOC molecular sieve adsorption materials are prepared by raw material of flyash | |
| CN104340989B (en) | A kind of hydrothermal synthesis method of 4A molecular sieves | |
| CN106276931A (en) | A kind of microwave synthesis method of lithium magnesium silicate | |
| CN106925239A (en) | A kind of novel drier and preparation method thereof | |
| CN104692410A (en) | Method for synthesizing A molecular sieve by crystallizing wet gel | |
| CN109336129A (en) | A kind of method of the illite without templated synthesis multi-stage porous ZSM-5 zeolite molecular sieve | |
| CN108654569A (en) | A kind of porous active silica gel preparation method | |
| CN106185975A (en) | A kind of method utilizing blast furnace slag to prepare molecular sieve crystal | |
| CN108128783A (en) | A kind of preparation method of 3A zeolite molecular sieves original powder | |
| CN103449469B (en) | A kind of NaY molecular sieve preparation method that improves stability | |
| CN111135787A (en) | Preparation method of improved 3A molecular sieve raw powder | |
| CN108726532B (en) | A kind of preparation method and applications of SSZ-24 molecular sieve | |
| CN107973316B (en) | Preparation method of hierarchical pore mordenite | |
| CN107459047A (en) | A kind of molecular sieve preparation method based on hemicellulose | |
| CN110127716A (en) | A kind of preparation method of multistage pore canal Y molecular sieve | |
| CN105347358A (en) | Preparation method of zeolite molecular sieve material having three-dimensional penetrating mesoporous multistage tunnel structure | |
| CN107055566A (en) | A kind of 3A molecular sieves and its processing technology | |
| CN107837785A (en) | A kind of preparation method of composite molecular screen defluorinating agent | |
| CN109110769A (en) | A kind of high dispersive silica and preparation method thereof | |
| CN109134734A (en) | A kind of preparation method of macroporous type strongly acidic styrene system ion exchange resin | |
| CN107855099A (en) | A kind of nano composite material to purify water |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A preparation method of 3A zeolite molecular sieve raw powder Effective date of registration: 20211229 Granted publication date: 20210409 Pledgee: China Construction Bank Corporation Wudi sub branch Pledgor: Shandong Lubei Enterprise Group Co. Registration number: Y2021980017007 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20220906 Granted publication date: 20210409 Pledgee: China Construction Bank Corporation Wudi sub branch Pledgor: Shandong Lubei Enterprise Group Co. Registration number: Y2021980017007 |