CN106276947B - A types and X-type mixed crystal zeolite, preparation method, preparation facilities and purposes - Google Patents

A types and X-type mixed crystal zeolite, preparation method, preparation facilities and purposes Download PDF

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Publication number
CN106276947B
CN106276947B CN201610675153.5A CN201610675153A CN106276947B CN 106276947 B CN106276947 B CN 106276947B CN 201610675153 A CN201610675153 A CN 201610675153A CN 106276947 B CN106276947 B CN 106276947B
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mixed crystal
types
type mixed
crystallization
preparation
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CN106276947A (en
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刘延东
崔宝
蔡转红
王东
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China Aluminum Shandong New Material Co ltd
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Aluminum Corp of China Ltd
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    • 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
    • C01B39/023—Preparation of physical mixtures or intergrowth products of zeolites chosen from group C01B39/04 or two or more of groups C01B39/14 - C01B39/48
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • C11D3/128—Aluminium silicates, e.g. zeolites
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/02—Inorganic compounds
    • C11D7/20—Water-insoluble oxides
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D9/00—Compositions of detergents based essentially on soap
    • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
    • C11D9/06—Inorganic compounds
    • C11D9/18—Water-insoluble compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • 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
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values

Abstract

The invention discloses a kind of A types and X-type mixed crystal zeolite, preparation method, preparation facilities and purposes, belong to zeolite technology field.This method includes that the water glass solution of the sodium aluminate solution and setting condition that impose a condition obtains the slurry of sodium aluminate solution and water glass solution according to the silica alumina ratio pulp of setting；The time for making the slurry crystallization of sodium aluminate solution and water glass solution persistently set under the crystallization temperature of setting, obtain crystallization product；Crystallization product after separation, washing, drying, obtains A types and X-type mixed crystal zeolite successively.The device includes slurrying tank, crystallization slot, drying device.The Lcc ＞ 70g/100g z of the A types and X-type mixed crystal zeolite that are prepared using this method and device, reach requirement of the hyperconcetration powder detergent formula to washing assisant Lcc indexs, therefore, can be used as washing assisant in hyperconcetration powder detergent.

Description

A types and X-type mixed crystal zeolite, preparation method, preparation facilities and purposes
Technical field
The present invention relates to zeolite technology field, more particularly to a kind of A types and X-type mixed crystal zeolite, preparation method, Preparation facilities and purposes.
Background technology
Type A zeolite is applied to as builder as substitute for phosphate in detergent production, is referred to as " Green Additives ", detergent zeolite Consumption figure accounts for the 85% of entire synthesis type A zeolite consumption figure.It is the maximum purposes of current 4A zeolites.X-type zeolite is a kind of important Micropore Si-Al zeolite, realized large-scale industrial application on chemical industry and petrochemical industry, be used as catalyst and adsorbent.
Referring to attached drawing 3, in the prior art, liquid nonionic surfactants (Lcc) index that detergent carries is in Between 38g/100g-z~58g/100g-z, requirement of the hyperconcetration powder detergent formula to washing assisant Lcc indexs is not achieved, i.e., ＞ 70g/100g-z.
Invention content
In view of this, a kind of A types of present invention offer and X-type mixed crystal zeolite, preparation method, preparation facilities, the A types And the Lcc index ＞ 70g/100g-z of X-type mixed crystal zeolite, reach requirement of the hyperconcetration powder formula to washing assisant, therefore, It can be used as washing assisant to be used for hyperconcetration powder detergent, thus more suitable for practicality.
In order to reach above-mentioned first purpose, the technical solution of A types and X-type mixed crystal zeolite provided by the invention is such as Under：
The Lcc ＞ 70g/100g-z of A types and X-type mixed crystal zeolite provided by the invention.
In order to reach above-mentioned second purpose, the skill of the preparation method of A types and X-type mixed crystal zeolite provided by the invention Art scheme is as follows：
The preparation method of A types and X-type mixed crystal zeolite provided by the invention includes the following steps：
The sodium aluminate solution of setting condition and the water glass solution of setting condition are obtained according to the silica alumina ratio pulp of setting The slurry of sodium aluminate solution and water glass solution；Wherein, in the sodium aluminate solution, Al2O3Concentration values ranging from 50g/L ~150g/L, α k value ranges are 1.4~3.5；In the water glass solution, SiO2Concentration values ranging from 50g/L~300g/ L, modulus value range is 1.0~3.5；The value range of the silica alumina ratio is 1.5~4.0；
The slurry crystallization of the sodium aluminate solution and water glass solution is set persistently to set under the crystallization temperature of setting Time obtains crystallization product；
The crystallization product after separation, washing, drying, obtains the A types and X-type mixed crystal zeolite successively.
It is further that following technical measures also can be used in the preparation method of A types and X-type mixed crystal zeolite provided by the invention It realizes.
Preferably, in the sodium aluminate solution, Al2O3Concentration values ranging from 60g/L~80g/L, α k value ranges are 2.0~3.2；In the water glass solution, SiO2Concentration values ranging from 150g/L~250g/L, modulus value range are 1.0 ~3.5；The value range of the silica alumina ratio is 1.5~2.0.
Preferably, the value range of the crystallization temperature is 70 DEG C~95 DEG C, the value model of the crystallization duration It encloses for 4h~10h.
Preferably, the value range of the crystallization temperature is 75 DEG C~85 DEG C, the value model of the crystallization duration It encloses for 5h~8h.
Preferably, the drying is spray drying.
In order to reach above-mentioned third purpose, the skill of the preparation facilities of A types and X-type mixed crystal zeolite provided by the invention Art scheme is as follows：
The preparation facilities of A types and X-type mixed crystal zeolite provided by the invention includes slurrying tank, crystallization slot, drying device,
The slurrying tank is used to house the slurry of sodium aluminate solution and water glass solution；Wherein, the sodium aluminate solution In, Al2O3Concentration values ranging from 50g/L~150g/L, α k value ranges are 1.4~3.5；In the water glass solution, SiO2 Concentration values ranging from 50g/L~300g/L, modulus value range are 1.0~3.5；
The crystallization slot is used to carry out crystallization to the slurry, obtains the crystallization product of the slurry；
The drying device obtains the A for the crystallization product successively after detaching, washing to be dried Type and X-type mixed crystal zeolite.
It is further that following technical measures also can be used in the preparation facilities of A types and X-type mixed crystal zeolite provided by the invention It realizes.
Preferably, the preparation facilities of the A types and X-type mixed crystal zeolite further includes heating device, the heating dress It sets for being heated to the crystallization slot so that the step of crystallization is realized under the crystallization temperature of setting.
Preferably, the drying device is spray-drying installation.
In order to reach above-mentioned 4th purpose, the technical side of the purposes of A types and X-type mixed crystal zeolite provided by the invention Case is as follows：
A types and X-type mixed crystal zeolite provided by the invention are used as the purposes of washing assisant in hyperconcetration powder detergent.
The Lcc of the A types and X-type mixed crystal zeolite that are prepared using preparation method provided by the invention and preparation facilities ＞ 70g/100g-z reach requirement of the hyperconcetration powder detergent formula to washing assisant Lcc indexs, therefore, can be super dense It is used as washing assisant in contracting powder detergent.
Description of the drawings
By reading the detailed description of hereafter preferred embodiment, various other advantages and benefit are common for this field Technical staff will become clear.Attached drawing only for the purpose of illustrating preferred embodiments, and is not considered as to the present invention Limitation.And throughout the drawings, the same reference numbers will be used to refer to the same parts.In the accompanying drawings：
Fig. 1 is the step flow chart of the preparation method of A types provided by the invention and X-type mixed crystal zeolite；
Fig. 2 is the substance variation signal during the preparation method of A types provided by the invention and X-type mixed crystal zeolite Figure；
Fig. 3 is the electron microscope of 4A zeolites in the prior art；
Fig. 4 is the electron microscope of A types provided by the invention and X-type mixed crystal zeolite；
Fig. 5 is the schematic diagram of the preparation facilities of A types provided by the invention and X-type mixed crystal zeolite.
Specific implementation mode
The present invention in order to solve the problems existing in the prior art, provides a kind of A types and X-type mixed crystal zeolite, its preparation side The Lcc index ＞ 70g/100g-z of method, preparation facilities, the A types and X-type mixed crystal zeolite, reach hyperconcetration powder formula to washing The requirement of auxiliary agent is washed, therefore, washing assisant can be used as to be used for hyperconcetration powder detergent, thus more suitable for practicality.
Inventor by largely testing, the study found that transiens zeolite between type A zeolite and X-type zeolite, I.e. the zeolite product with A types, X-type mixed crystal, Lcc can meet the requirement of Lcc ＞ 70g/100g-z or more.Study carefully its original Because being at crystallization initial stage, two kinds of crystal occur simultaneously, and two kinds of crystal are grown up and interfered with each other simultaneously in crystallization process, ultimately form There are two types of crystal form, the rough products of particle surface, referring to attached drawing 4, due to its particle surface for a kind of particle tool Particularity causes the raising of its Lcc index.
It is of the invention to reach the technological means and effect that predetermined goal of the invention is taken further to illustrate, below in conjunction with Attached drawing and preferred embodiment, to propose according to the present invention A types and X-type mixed crystal zeolite, preparation method, preparation facilities and Purposes, specific implementation mode, structure, feature and its effect are described in detail as after.In the following description, a different " implementation What example " or " embodiment " referred to is not necessarily the same embodiment.In addition, the special characteristic, structure in one or more embodiments or spy Point can be combined by any suitable form.
The terms "and/or", only a kind of incidence relation of description affiliated partner, indicates that there may be three kinds of passes System, for example, A and/or B, is specifically interpreted as：Can include A and B simultaneously, can be with individualism A, it can also individualism B can have above-mentioned three kinds of any case.
The Lcc ＞ 70g/100g-z of A types and X-type mixed crystal zeolite provided by the invention.
Referring to attached drawing 1 and attached drawing 2, the preparation method of A types and X-type mixed crystal zeolite provided by the invention includes following step Suddenly：
Step S1：The sodium aluminate solution of setting condition and the water glass solution of setting condition are starched according to the silica alumina ratio of setting Change, obtains the slurry of sodium aluminate solution and water glass solution；Wherein, in sodium aluminate solution, Al2O3Concentration values are ranging from 50g/L~150g/L, α k value ranges are 1.4~3.5；In water glass solution, SiO2Concentration values ranging from 50g/L~ 300g/L, modulus value range are 1.0~3.5；The value range of silica alumina ratio is 1.5~4.0；
Step S2：The slurry crystallization of sodium aluminate solution and water glass solution is set persistently to set under the crystallization temperature of setting Time, obtain crystallization product；
Step S3：Crystallization product after separation, washing, drying, obtains A types and X-type mixed crystal zeolite successively.
Wherein, in sodium aluminate solution, Al2O3Concentration values ranging from 60g/L~80g/L, α k value ranges be 2.0~ 3.2；In water glass solution, SiO2Concentration values ranging from 150g/L~250g/L, modulus value range are 1.0~3.5；Sial The value range of ratio is 1.5~2.0.
Wherein, the value range of crystallization temperature is 70 DEG C~95 DEG C, and the value range of crystallization duration is 4h~10h.
Wherein, the value range of crystallization temperature is 75 DEG C~85 DEG C, and the value range of crystallization duration is 5h~8h.
Wherein, dry for spray drying.
Referring to attached drawing 5, the preparation facilities of A types and X-type mixed crystal zeolite provided by the invention includes slurrying tank 3, crystallization Slot 4, drying device.Slurrying tank 3 is used to house the slurry 5 of sodium aluminate solution and water glass solution；Wherein, sodium aluminate solution 7 In (the first container 1 is for housing sodium aluminate solution), Al2O3Concentration values ranging from 50g/L~150g/L, α k value ranges are 1.4~3.5；In water glass solution 8 (second container 2 is for housing water glass solution), SiO2Concentration values ranging from 50g/L~ 300g/L, modulus value range are 1.0~3.5；The value range of silica alumina ratio is 1.5~4.0；Crystallization slot 4 is used for slurry 6 Crystallization is carried out, the crystallization product of sodium aluminate solution and water glass solution is obtained；Drying device is used for successively by separation, washing Crystallization product deformity drying afterwards, obtains A types and X-type mixed crystal zeolite.
Wherein, the preparation facilities of A types and X-type mixed crystal zeolite further includes heating device (not shown), heating dress It sets for being heated to crystallization slot 4 so that the step of crystallization is realized under the crystallization temperature of setting.
Wherein, drying device is spray-drying installation.
A types and X-type mixed crystal zeolite provided by the invention are used as the purposes of washing assisant in hyperconcetration powder detergent.
The Lcc of the A types and X-type mixed crystal zeolite that are prepared using preparation method provided by the invention and preparation facilities ＞ 70g/100g-z reach requirement of the hyperconcetration powder detergent formula to washing assisant Lcc indexs, therefore, can be super dense It is used as washing assisant in contracting powder detergent.
Examples 1 to 21
Although preferred embodiments of the present invention have been described, it is created once a person skilled in the art knows basic Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as It selects embodiment and falls into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art God and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies Within, then the present invention is also intended to include these modifications and variations.

Claims (5)

  1. The preparation method of 1.A types and X-type mixed crystal zeolite, which is characterized in that include the following steps：
    The sodium aluminate solution of setting condition and the water glass solution of setting condition obtain aluminic acid according to the silica alumina ratio pulp of setting The slurry of sodium solution and water glass solution；Wherein, in the sodium aluminate solution, Al2O3Concentration values ranging from 50g/L~ 150g/L, α k value ranges are 1.4~3.5；In the water glass solution, SiO2Concentration values ranging from 50g/L~300g/L, Modulus value range is 1.0~3.5；The value range of the silica alumina ratio is 1.5~4.0；
    The time for making the slurry crystallization of the sodium aluminate solution and water glass solution persistently set under the crystallization temperature of setting, Obtain crystallization product；
    The crystallization product after separation, washing, drying, obtains the A types and X-type mixed crystal zeolite, the A types successively And the Lcc ＞ 70g/100g-z of X-type mixed crystal zeolite.
  2. 2. the preparation method of A types according to claim 1 and X-type mixed crystal zeolite, which is characterized in that
    In the sodium aluminate solution, Al2O3Concentration values ranging from 60g/L~80g/L, α k value ranges are 2.0~3.2；It is described In water glass solution, SiO2Concentration values ranging from 150g/L~250g/L, modulus value range are 1.0~3.5；The sial The value range of ratio is 1.5~2.0.
  3. 3. the preparation method of A types according to claim 1 and X-type mixed crystal zeolite, which is characterized in that the crystallization temperature The value range of degree is 70 DEG C~95 DEG C, and the value range of the crystallization duration is 4h~10h.
  4. 4. the preparation method of A types according to claim 3 and X-type mixed crystal zeolite, which is characterized in that the crystallization temperature The value range of degree is 75 DEG C~85 DEG C, and the value range of the crystallization duration is 5h~8h.
  5. 5. the preparation method of A types according to claim 1 and X-type mixed crystal zeolite, which is characterized in that the drying is Spray drying.
CN201610675153.5A 2016-08-16 2016-08-16 A types and X-type mixed crystal zeolite, preparation method, preparation facilities and purposes Active CN106276947B (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1420845A (en) * 2000-03-17 2003-05-28 Pq控股公司 Process for manufacture of zeolites and zeolite mixtures having enhanced cation exchange properties, products produced thereby, and detergent compositions formulated therewith

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1420845A (en) * 2000-03-17 2003-05-28 Pq控股公司 Process for manufacture of zeolites and zeolite mixtures having enhanced cation exchange properties, products produced thereby, and detergent compositions formulated therewith

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Effective date of registration: 20230912

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