CN1699171A - Manufacturing process of 4A type molecular sieve primary powder with low bulk density - Google Patents

Manufacturing process of 4A type molecular sieve primary powder with low bulk density Download PDF

Info

Publication number
CN1699171A
CN1699171A CN 200510043515 CN200510043515A CN1699171A CN 1699171 A CN1699171 A CN 1699171A CN 200510043515 CN200510043515 CN 200510043515 CN 200510043515 A CN200510043515 A CN 200510043515A CN 1699171 A CN1699171 A CN 1699171A
Authority
CN
China
Prior art keywords
pulp
crystallization
manufacturing process
type molecular
primary powder
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.)
Pending
Application number
CN 200510043515
Other languages
Chinese (zh)
Inventor
韩辉
王树栋
王忠慧
李鹏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SHANDONG ALUMINIUM INDUSTRY Co Ltd
Original Assignee
SHANDONG ALUMINIUM INDUSTRY Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by SHANDONG ALUMINIUM INDUSTRY Co Ltd filed Critical SHANDONG ALUMINIUM INDUSTRY Co Ltd
Priority to CN 200510043515 priority Critical patent/CN1699171A/en
Publication of CN1699171A publication Critical patent/CN1699171A/en
Pending legal-status Critical Current

Links

Images

Landscapes

  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Glass Compositions (AREA)

Abstract

The invention relates to a manufacturing process of 4A type molecular sieve primary powder with low bulk density which comprises proportioning, pulping, crystallizing, separating crystal and washing, wherein the reaction system is controlled to be 2.7-4.0Na2O * Al2O3 * 1.8-2.1 SiO2 * 110-170H2O. By employing the heat synthesis of sodium aluminate solution with sodium silicate and reducing water-sodium ratio, the reactant concentration of the synthesizing system can be increased.

Description

Low heap is than the manufacturing process of 4A type molecular screen primary powder
Technical field
The present invention relates to the manufacturing process of a kind of low heap, be the synthetic technology of 4A type molecular sieve than 4A type molecular screen primary powder.
Background technology
Zeolite molecular sieve has selects absorption, shape selective catalysis and ion-exchange three big characteristics, multiple industrial circles such as that pure system, air separation, the oil that is widely used in depth drying, Sweet natural gas and the hydrogen of industrial gasses and liquid takes off is cured, double glazing and catalytic cracking.Wherein A type molecular sieve is a kind of multi-functional, broad-spectrum product, utilizes its ion exchanging function, 4A molecular sieve (Na 2OAl 2O 32SiO 24.5H 2O) can be used as detergent builder, the 4A molecular sieve also has adsorptivity simultaneously, adsorbable molecular diameter is less than the molecule of 4 dusts, as water molecules etc., air, oil, carbonic acid gas, organic solvent etc. are carried out depth drying, be widely used in building, chemistry, chemical industry and the daily life, the 4A molecular sieve is again the raw material of preparation 3A, 5A molecular sieve.The multifunctionality of 4A molecular sieve makes the use range of A type molecular sieve constantly obtain developing, and Application Areas is constantly developed.
In modern double glazing production, the general method that adopts fully-closed, vacuumizes, in molecular sieve filled aluminum pipe around double glazing, this technology proposes more and more high requirement to the performance of molecular screen primary powder: bulk density is little, loading capacity is big, low, the good product mobility of dust in the moulding process.4A molecular screen primary powder how to produce this performance is the new problem that needs research.
Summary of the invention
The object of the present invention is to provide a kind of manufacturing process of improved 4A type molecular screen primary powder, the 4A type molecular screen primary powder heap of manufacturing is than low, and loading capacity is big.
Low heap of the present invention through making after batching, pulp, crystallization, isolation of crystalline and the washing, is prepared burden by sodium aluminate solution and service water glass successively than the manufacturing process of 4A type molecular screen primary powder, and pulp, crystallization system are controlled to be: 2.7～4.0Na 2OAl 2O 31.8～2.1SiO 2110～170H 2O.
Add directed agents and promote reaction when pulp, directed agents is prepared according to following method:
The preparation alumina content is that sodium aluminate solution and the silica content of 30～60g/l is that 160～200g/l, sodium oxide content are the water glass of 50～80g/l, presses Na 2O and Al 2O 3Mol ratio (10～18): 1, SiO 2And Al 2O 3Mol ratio be (8～14): 1, H 2O and Al 2O 3Mol ratio be (280～350): 1 ratio has been calculated the consumption of sodium aluminate solution, water glass, sodium hydroxide and water, attemperation is 40～60 ℃, under brute force stirs, four kinds of raw materials are mixed, continue to stir after 10～60 minutes and left standstill 45～100 hours, promptly get directed agents.
It is suitable that the add-on of directed agents is controlled to be 1 of reaction soln volume～20 ‰.
The pulp reaction conditions is: the pulp temperature is 50～70 ℃, and the pulp time is 10～20 minutes.
The crystallization condition is: crystallization temperature is 70～93 ℃, and crystallization time is 1～1.5 hour.
Other control condition of whole process, as press filtration separation, crystal washing and drying etc., identical with the manufacture method of 4A zeolite, directly the technology of following conventional lines gets final product, and repeats no more.
The present invention has adopted sodium aluminate solution and water glass hydrothermal synthesis method, by reducing the reactant concn of water-sodium ratio, raising synthetic system, adopt short crystallization time to produce heap than the 4A molecular screen primary powder little, that loading capacity is big (pine dress heap is than 0.22～0.37g/ml, static water-intake rate＞26.5%), and product surface is hard smooth, dust is low in the filling process, good flowing properties, it is dedicated molecular sieve used to be particularly suitable for doing double glazing.Manufacturing process of the present invention is simple and easy to do, and production cost is low, and is with short production cycle, product solid content height, and the output height has reached intended purposes, has satisfied the performance requriements of product.
Description of drawings
Fig. 1, process flow diagram of the present invention.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
The preparation of directed agents: the preparation alumina content is that sodium aluminate solution and the silica content of 45g/l is that 180g/l, sodium oxide content are the water glass (ortho-water glass gets final product, and general modulus is 3.0～3.3) of 65g/l, presses Na 2O and Al 2O 3Mol ratio 15: 1, SiO 2And Al 2O 3Mol ratio be 10: 1, H 2O and Al 2O 3Mol ratio be the consumption that 300: 1 ratio has been calculated sodium aluminate solution, water glass, sodium hydroxide and water, attemperation is 45 ℃, under brute force stirs four kinds of raw materials is mixed, and continues to stir to leave standstill after 48 hours after 30 minutes promptly to get directed agents.
Low heap of the present invention is prepared burden by sodium aluminate solution and service water glass than the manufacturing process of 4A type molecular screen primary powder, makes after pulp, crystallization, isolation of crystalline, washing and drying, and wherein, pulp, crystallization system are controlled to be: 2.8Na 2OAl 2O 32SiO 2165H 2O.
2 ‰ directed agents that add the reaction soln volume during pulp;
The pulp reaction conditions is controlled to be: the pulp temperature is 53 ± 3 ℃, and the pulp time is 10 minutes;
The crystallization condition is controlled to be: crystallization temperature is 91 ± 2 ℃, and crystallization time is 1.2 hours.
Embodiment 2
The preparation of directed agents: the preparation alumina content is that sodium aluminate solution and the silica content of 48g/l is that 178g/l, sodium oxide content are the water glass of 66g/l, presses Na 2O and Al 2O 3Mol ratio 16: 1, SiO 2And Al 2O 3Mol ratio be 9: 1, H 2O and Al 2O 3Mol ratio be the consumption that 280: 1 ratio has been calculated sodium aluminate solution, water glass, sodium hydroxide and water, attemperation is 47 ℃, under brute force stirs four kinds of raw materials is mixed, and continues to stir after 25 minutes and leaves standstill 49 hours, promptly gets directed agents.
Low heap of the present invention is prepared burden by sodium aluminate solution and service water glass than the manufacturing process of 4A type molecular screen primary powder, makes after pulp, crystallization, isolation of crystalline, washing and drying, and wherein, pulp, crystallization system are controlled to be: 3.6Na 2OAl 2O 31.8SiO 2130H 2O.
4 ‰ directed agents that add the reaction soln volume during pulp;
The pulp reaction conditions is controlled to be: the pulp temperature is 60 ± 3 ℃, and the pulp time is 15 minutes;
The crystallization condition is controlled to be: crystallization temperature is 75 ± 2 ℃, and crystallization time is 1.5 hours.
Embodiment 3
The preparation of directed agents: the preparation alumina content is that sodium aluminate solution and the silica content of 43g/l is that 185g/l, sodium oxide content are the water glass of 63g/l, presses Na 2O and Al 2O 3Mol ratio 11: 1, SiO 2And Al 2O 3Mol ratio be 12: 1, H 2O and Al 2O 3Mol ratio be the consumption that 330: 1 ratio has been calculated sodium aluminate solution, water glass, sodium hydroxide and water, attemperation is 44 ℃, under brute force stirs four kinds of raw materials is mixed, and continues to stir after 27 minutes and leaves standstill 50 hours, promptly gets directed agents;
Low heap of the present invention is prepared burden by sodium aluminate solution and service water glass than the manufacturing process of 4A type molecular screen primary powder, makes after pulp, crystallization, isolation of crystalline, washing and drying, and wherein, pulp, crystallization system are controlled to be: 3.8Na 2OAl 2O 32.1SiO 2120H 2O.
5 ‰ directed agents that add the reaction soln volume during pulp;
The pulp reaction conditions is controlled to be: the pulp temperature is 54 ± 3 ℃, and the pulp time is 18 minutes;
The crystallization condition is controlled to be: crystallization temperature is 80 ± 1 ℃, and crystallization time is 1.1 hours.
Embodiment 4
Low heap of the present invention is prepared burden by sodium aluminate solution and service water glass than the manufacturing process of 4A type molecular screen primary powder, makes after pulp, crystallization, isolation of crystalline, washing and drying, and wherein, pulp, crystallization system are controlled to be: 2.7Na 2OAl 2O 31.8SiO 2170H 2O.
8 ‰ directed agents that add the reaction soln volume during pulp;
The pulp reaction conditions is controlled to be: the pulp temperature is 57 ± 2 ℃, and the pulp time is 14 minutes;
The crystallization condition is controlled to be: crystallization temperature is 90 ± 2 ℃, and crystallization time is 1.3 hours.
Other is with embodiment 1.
Embodiment 5
The preparation of directed agents: the preparation alumina content is that sodium aluminate solution and the silica content of 55g/l is that 200g/l, sodium oxide content are the water glass of 65g/l, presses Na 2O and Al 2O 3Mol ratio 13: 1, SiO 2And Al 2O 3Mol ratio be 13: 1, H 2O and Al 2O 3Mol ratio be the consumption that 310: 1 ratio has been calculated sodium aluminate solution, water glass, sodium hydroxide and water, attemperation is 52 ℃, under brute force stirs four kinds of raw materials is mixed, and continues to stir after 25 minutes and leaves standstill 60 hours, promptly gets directed agents.
Low heap of the present invention is prepared burden by sodium aluminate solution and service water glass than the manufacturing process of 4A type molecular screen primary powder, makes after pulp, crystallization, isolation of crystalline, washing and drying, and wherein, pulp, crystallization system are controlled to be: 2.9Na 2OAl 2O 31.9SiO 2140H 2O.
3 ‰ directed agents that add the reaction soln volume during pulp;
The pulp reaction conditions is controlled to be: the pulp temperature is 58 ± 2 ℃, and the pulp time is 15 minutes;
The crystallization condition is controlled to be: crystallization temperature is 92 ± 1 ℃, and crystallization time is 1 hour.
Embodiment 6
The preparation of directed agents: the preparation alumina content is that sodium aluminate solution and the silica content of 43g/l is that 190g/l, sodium oxide content are the water glass of 76g/l, presses Na 2O and Al 2O 3Mol ratio 12: 1, SiO 2And Al 2O 3Mol ratio be 12: 1, H 2O and Al 2O 3Mol ratio be the consumption that 310: 1 ratio has been calculated sodium aluminate solution, water glass, sodium hydroxide and water, attemperation is 48 ℃, under brute force stirs four kinds of raw materials is mixed, and continues to stir after 50 minutes and leaves standstill 80 hours, promptly gets directed agents;
Low heap of the present invention is prepared burden by sodium aluminate solution and service water glass than the manufacturing process of 4A type molecular screen primary powder, makes after pulp, crystallization, isolation of crystalline, washing and drying, and wherein, pulp, crystallization system are controlled to be: 3.0Na 2OAl 2O 32SiO 2150H 2O.
7 ‰ directed agents that add the reaction soln volume during pulp;
The pulp reaction conditions is controlled to be: the pulp temperature is 56 ± 2 ℃, and the pulp time is 16 minutes;
The crystallization condition is controlled to be: crystallization temperature is 92 ± 1 ℃, and crystallization time is 1.2 hours.
Embodiment 7
The preparation of directed agents: the preparation alumina content is that sodium aluminate solution and the silica content of 43g/l is that 185g/l, sodium oxide content are the water glass of 63g/l, presses Na 2O and Al 2O 3Mol ratio 11: 1, SiO 2And Al 2O 3Mol ratio be 12: 1, H 2O and Al 2O 3Mol ratio be the consumption that 330: 1 ratio has been calculated sodium aluminate solution, water glass, sodium hydroxide and water, attemperation is 44 ℃, under brute force stirs four kinds of raw materials is mixed, and continues to stir after 27 minutes and leaves standstill 50 hours, promptly gets directed agents;
Low heap of the present invention is prepared burden by sodium aluminate solution and service water glass than the manufacturing process of 4A type molecular screen primary powder, makes after pulp, crystallization, isolation of crystalline, washing and drying, and wherein, pulp, crystallization system are controlled to be: 3.3Na 2OAl 2O 31.9SiO 2140H 2O.
3 ‰ directed agents that add the reaction soln volume during pulp;
The pulp reaction conditions is controlled to be: the pulp temperature is 58 ± 2 ℃, and the pulp time is 15 minutes;
The crystallization condition is controlled to be: crystallization temperature is 88 ± 1 ℃, and crystallization time is 1 hour.
Embodiment 8
The preparation of directed agents: the preparation alumina content is that sodium aluminate solution and the silica content of 48g/l is that 178g/l, sodium oxide content are the water glass of 66g/l, presses Na 2O and Al 2O 3Mol ratio 16: 1, SiO 2And Al 2O 3Mol ratio be 9: 1, H 2O and Al 2O 3Mol ratio be the consumption that 280: 1 ratio has been calculated sodium aluminate solution, water glass, sodium hydroxide and water, attemperation is 47 ℃, under brute force stirs four kinds of raw materials is mixed, and continues to stir after 25 minutes and leaves standstill 49 hours, promptly gets directed agents.
Low heap of the present invention is prepared burden by sodium aluminate solution and service water glass than the manufacturing process of 4A type molecular screen primary powder, makes after pulp, crystallization, isolation of crystalline, washing and drying, and wherein, pulp, crystallization system are controlled to be: 2.8Na 2OAl 2O 32SiO 2150H 2O.
10 ‰ directed agents that add the reaction soln volume during pulp;
The pulp reaction conditions is controlled to be: the pulp temperature is 55 ± 2 ℃, and the pulp time is 15 minutes;
The crystallization condition is controlled to be: crystallization temperature is 89 ± 2 ℃, and crystallization time is 1.3 hours.
Embodiment 9
The preparation of directed agents: the preparation alumina content is that sodium aluminate solution and the silica content of 43g/l is that 190g/l, sodium oxide content are the water glass of 76g/l, presses Na 2O and Al 2O 3Mol ratio 12: 1, SiO 2And Al 2O 3Mol ratio be 12: 1, H 2O and Al 2O 3Mol ratio be the consumption that 310: 1 ratio has been calculated sodium aluminate solution, water glass, sodium hydroxide and water, attemperation is 48 ℃, under brute force stirs four kinds of raw materials is mixed, and continues to stir after 50 minutes and leaves standstill 80 hours, promptly gets directed agents;
Low heap of the present invention is prepared burden by sodium aluminate solution and service water glass than the manufacturing process of 4A type molecular screen primary powder, makes after pulp, crystallization, isolation of crystalline, washing and drying, and wherein, pulp, crystallization system are controlled to be: 3.0Na 2OAl 2O 32SiO 2150H 2O.
7 ‰ directed agents that add the reaction soln volume during pulp;
The pulp reaction conditions is controlled to be: the pulp temperature is 66 ± 2 ℃, and the pulp time is 16 minutes;
The crystallization condition is controlled to be: crystallization temperature is 92 ± 1 ℃, and crystallization time is 1.2 hours.

Claims (5)

1, a kind of low heap is than the manufacturing process of 4A type molecular screen primary powder, successively through making after batching, pulp, crystallization, isolation of crystalline and the washing, it is characterized in that being prepared burden by sodium aluminate solution and service water glass, pulp, crystallization system are controlled to be: 2.7～4.0Na 2OAl 2O 31.8～2.1 SiO 2110～170H 2O.
2, low heap according to claim 1 adds directed agents than the manufacturing process of 4A type molecular screen primary powder when it is characterized in that pulp, and directed agents is prepared according to following method:
The preparation alumina content is that sodium aluminate solution and the silica content of 30～60g/l is that 160～200g/l, sodium oxide content are the water glass of 50～80g/l, presses Na 2O and Al 2O 3Mol ratio (10～18): 1, SiO 2And Al 2O 3Mol ratio be (8～14): 1, H 2O and Al 2O 3Mol ratio be (280～350): 1 ratio has been calculated the consumption of sodium aluminate solution, water glass, sodium hydroxide and water, attemperation is 40～60 ℃, under brute force stirs, four kinds of raw materials are mixed, continue to stir after 10～60 minutes and left standstill 45～100 hours, promptly get directed agents.
3, low heap according to claim 2 is than the manufacturing process of 4A type molecular screen primary powder, and the add-on that it is characterized in that directed agents is 1 of reaction soln volume～20 ‰.
4, low heap according to claim 3 is than the manufacturing process of 4A type molecular screen primary powder, and it is characterized in that the pulp reaction conditions is: the pulp temperature is 50～70 ℃, and the pulp time is 10～20 minutes.
5, according to claim 1,2, the 3 or 4 described low heaps manufacturing process than 4A type molecular screen primary powder, it is characterized in that the crystallization condition is: crystallization temperature is 70～93 ℃, and crystallization time is 1～1.5 hour.
CN 200510043515 2005-05-12 2005-05-12 Manufacturing process of 4A type molecular sieve primary powder with low bulk density Pending CN1699171A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200510043515 CN1699171A (en) 2005-05-12 2005-05-12 Manufacturing process of 4A type molecular sieve primary powder with low bulk density

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 200510043515 CN1699171A (en) 2005-05-12 2005-05-12 Manufacturing process of 4A type molecular sieve primary powder with low bulk density

Publications (1)

Publication Number Publication Date
CN1699171A true CN1699171A (en) 2005-11-23

Family

ID=35475456

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 200510043515 Pending CN1699171A (en) 2005-05-12 2005-05-12 Manufacturing process of 4A type molecular sieve primary powder with low bulk density

Country Status (1)

Country Link
CN (1) CN1699171A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103030157A (en) * 2011-09-30 2013-04-10 广州市恒邦精细化工有限公司 Superfine molecular sieve original powder and preparation method thereof
CN106517355A (en) * 2016-11-11 2017-03-22 西安科技大学 Ultrasonic preparation method of magnetic 4A molecular sieve
CN107311192A (en) * 2017-07-26 2017-11-03 东北大学 The method that the hot method processing Bayer process red mud of the step alkali of andradite one produces 4A zeolites
CN109678173A (en) * 2019-02-26 2019-04-26 郑州雪山实业股份有限公司 With the process of the sodium metaaluminate waste liquid synthesis 4A molecular sieve containing potassium
CN112707838A (en) * 2019-10-25 2021-04-27 中国石油化工股份有限公司 Method for recovering N, N-dimethylacetamide

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103030157A (en) * 2011-09-30 2013-04-10 广州市恒邦精细化工有限公司 Superfine molecular sieve original powder and preparation method thereof
CN103030157B (en) * 2011-09-30 2016-05-25 广州市恒邦精细化工有限公司 Former powder of a kind of superfine molecular sieves and preparation method thereof
CN106517355A (en) * 2016-11-11 2017-03-22 西安科技大学 Ultrasonic preparation method of magnetic 4A molecular sieve
CN107311192A (en) * 2017-07-26 2017-11-03 东北大学 The method that the hot method processing Bayer process red mud of the step alkali of andradite one produces 4A zeolites
CN109678173A (en) * 2019-02-26 2019-04-26 郑州雪山实业股份有限公司 With the process of the sodium metaaluminate waste liquid synthesis 4A molecular sieve containing potassium
CN112707838A (en) * 2019-10-25 2021-04-27 中国石油化工股份有限公司 Method for recovering N, N-dimethylacetamide
CN112707838B (en) * 2019-10-25 2022-12-09 中国石油化工股份有限公司 Method for recovering N, N-dimethylacetamide

Similar Documents

Publication Publication Date Title
CN1730391A (en) Microwave method for synthesizing nanometer silicate basic hole material
CN1699171A (en) Manufacturing process of 4A type molecular sieve primary powder with low bulk density
CN1676210A (en) High active calcium-base CO2 absorbent and its preparing method
CN1944254A (en) Double micro pore high silicon composite molecular sieve and its preparing method
CN1291917C (en) Method for synthesizing Y-zeolite composite material
CN105271299B (en) A kind of preparation method of the zeolites of mesoporous ZSM 5
CN1724141A (en) Process for preparing adsorbent of molecular sieve with high adsorption value fluorite
CN101066766A (en) Zeolite molecular sieve and its prepn process with palygorskite as material
JP2007050403A (en) Method for producing catalyst to be used for p-xylene production by toluene form selective alkylation
CN1033503C (en) Process for preparation of small crystal grain Na Y molecular sieve
CN1205122C (en) Process for synthesizing ZSM-5 molecular sieve
CN1683246A (en) Process for preparing NaY molecular sieve
CN1749161A (en) Hard template synthetic composite hole zeolite molecular sieve and its preparing method
CN1737085A (en) LTA and FAU molecular screen nanocrystalline preparation method
CN1093512C (en) Synthesizing method for high-silicon mordenite
CN106946268A (en) A kind of MOR/ZSM-35 composite molecular screens and its synthetic method
CN1631780A (en) Method for producing 4A molecular sieve by using waste liquid of NaY molecular sieve production
CN1116229C (en) Synthesis method of high-silicon mordenite
CN1724361A (en) Tech. for mfg. high stack ratio 4A type molecular sieve ortho-powder
CN1915513A (en) Method for preparing catalyst of para xylene through methylation of toluene
CN1191198C (en) Nano-class molecular sieve and its synthesizing process
CN1289398C (en) 4A zeolite, manufacture method and use thereof
CN1058681C (en) Process of producing fine-grain model. A zeolite
CN1915514A (en) Method for preparing catalyst of para xylene through form selected methylation of toluene
CN1240817C (en) Technical method for producing P type zeolite utilized in bath by using alkali solution to activate bentonite under high temperature and high pressure

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C12 Rejection of a patent application after its publication
RJ01 Rejection of invention patent application after publication