CN106047182A - Multi-metal phosphate adhesive and preparation method thereof - Google Patents
Multi-metal phosphate adhesive and preparation method thereof Download PDFInfo
- Publication number
- CN106047182A CN106047182A CN201610395445.3A CN201610395445A CN106047182A CN 106047182 A CN106047182 A CN 106047182A CN 201610395445 A CN201610395445 A CN 201610395445A CN 106047182 A CN106047182 A CN 106047182A
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- Prior art keywords
- adhesive
- metal phosphates
- many metal
- colloid
- metal oxide
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J1/00—Adhesives based on inorganic constituents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a multi-metal phosphate adhesive which is prepared from the following raw materials in parts by weight: 40-60 parts of multi-metal phosphate colloid, 40-60 parts of deionized water, 1-2 parts of organic silicon water repellent, 2-3 parts of high polymer emulsion and 2-5 parts of inorganic filler powder. Compared with the prior art, the invention provides a method for preparing the polymetallic phosphate colloid by reacting phosphoric acid with polymetallic oxide/hydroxide, and the polymetallic phosphate adhesive is prepared by adding organosilicon water repellent, high molecular polymer emulsion, active inorganic filler and the like in different proportions on the basis of the colloid. The system of the adhesive is acidic, and the hydroxide corresponding to the metal cation has low solubility in water, so that the path of alkali return can be effectively cut off, and the problem of alkali reversion of the plate in the application process is solved.
Description
Technical field
The invention belongs to adhesive techniques field, be specifically related to a kind of many metal phosphates adhesive and preparation method thereof.
Background technology
Traditionally, use the pearlite heat-insulation plate that waterglass is prepared as bonding agent, owing to its cost is low, production
Technique is simple, high insulating effect, and has the fireproof heat insulating characteristic of uniqueness, becomes the hot product substituting organic heat-insulating plate.
For being main bonding agent with waterglass and the relevant report that improves caking agent series is occurring the most in a large number, but
Owing to this material of waterglass self has high concentration Na ion, high concentration Na ion can make the Si-O-Si key of adhesive action
Reversible degraded occurs.Along with the process of this reversible degraded, during practical implementation, inevitably produce two
The most serious consequence: 1. weatherability is poor, there is bigger loss in sheet material mechanics of materials intensity in use for some time;2. go out
The most serious accumulation of salt in the surface soil problem, Si-O-Si key is after fracture, and metastable Na ion starts to have great animal migration and go out
The accumulation of salt in the surface soil phenomenon of existing wall face, the appearance of accumulation of salt in the surface soil phenomenon then can cause the coating of metope to occur that mottled even locality comes off.
Tsing-Hua University Bao Jie et al. once did correlational study exclusively for construction wall accumulation of salt in the surface soil problem, and thought accumulation of salt in the surface soil problem
Occur that attribution is two big steps: 1. the sodium silicate in body of wall generates precipitated calcium silicate and sodium hydroxide with Calx effect;2. hydrogen
Sodium oxide CO in surface of wall absorbs air2And form main component basic carbonate sodium and the sodium carbonate of accumulation of salt in the surface soil thing.And water
The preparation process of glass is exactly the Na of the high alkalinity being bound up with high-concentration sodium hydroxide and fine silica powder2O·nSiO2
Colloid, the high alkalinity environment of system self and the existence of high concentration Na ion make this adhesive of waterglass be provided with natural returning
The attribute of alkali.Therefore, to avoid inorganic adhesive to occur, accumulation of salt in the surface soil phenomenon then must be cut off from principle and the path of the accumulation of salt in the surface soil occurs,
First, whole adhesive system should be neutral or acid;Secondly, the cation of adhesive can not be the alkali that dissolubility is high
Metal ion.
Summary of the invention
The technical problem to be solved in the present invention be traditional waterglass bonding agent due to system self high alkalinity environment with
The existence of high concentration Na ion makes this adhesive of waterglass be provided with the attribute of the natural accumulation of salt in the surface soil, and weatherability is poor, and sheet material exists
After using a period of time, there is bigger loss in mechanics of materials intensity, and for solving the problems referred to above, the present invention provides a kind of many metals
Phosphate adhesive and preparation method thereof.
It is an object of the invention to realize in the following manner:
A kind of many metal phosphates adhesive, is made up of the raw material of following weight portion: many metal phosphates colloid 40-60 part, goes
Ionized water 40-60 part, organosilicon moisture repellent 1-2 part, macromolecule emulsion 2-3 part, inorganic filler powder body 2-5 part.
Described many metal phosphates colloid includes aluminium hydroxide, II A family metal oxide, transition metal oxide, quality
Mark is phosphoric acid solution and the deionized water of 80%;Wherein, aluminium hydroxide, II A family metal oxide and transition metal oxide
Mol ratio be n1:n2:n3=(50-100): (0-50): (0-50), mass fraction be 80% phosphoric acid solution in institute's phosphoric acid
Molal quantity be: n4=3n1+2n2+2n3, the quality of deionized water is the 5%-20% of many metal phosphates colloid gross mass.
Described aluminium hydroxide is the powder body that purity is more than 95%.
Described II A family metal oxide is at least one in BeO, MgO, CaO, SrO and BaO, and purity is more than 98%, grain
Degree is less than 800 mesh.
Described II A family metal oxide is at least one in MgO and CaO.
Described transition metal oxide is FeO, CuO, ZnO, Cr2O3, MnO2And ZrO2In at least one, purity is more than
98%, granularity is less than 800 mesh.
Described organosilicon moisture repellent is methyl silicon sodium alcoholate, in isobutyl group sodium silanolate or isooctyltriethoxysilane
Kind.
Described macromolecule emulsion is styrene-acrylic emulsion, JS emulsion, the one in emulsified asphalt or modified acrylic acid emulsion.
Described inorganic filler powder body is at least one in white carbon, ultrafine kaolin and Ultra-fine Bentonite.
Concrete operation step is:
A. the preparation of many metal phosphates colloid: weigh aluminium hydroxide, II A family metal oxide and transition metal oxide, mixed
There-necked flask is put into after closing uniformly;Weighing phosphoric acid solution again, and be slowly added in there-necked flask by phosphoric acid solution, limit edged stirs
Mix;To there-necked flask reload temperature meter, agitator and reflux condensing tube respectively, then there-necked flask is put into the constant temperature of 80-100 DEG C
Heated and stirred in oil bath, question response system temperature stably starts timing later, adds deionized water stirring after reaction 20-40min
Uniformly;
B. the preparation of many metal phosphates adhesive: weigh many metal phosphates colloid, adds deionized water, adds and weigh
Organosilicon moisture repellent, macromolecule emulsion and inorganic filler powder body, in stirrer for mixing uniformly.
Relative to prior art, the present invention propose use phosphoric acid and poly-metal deoxide/hydroxide react prepare many
The method of metal phosphate colloid, and to based on this kind of colloid by add the organosilicon moisture repellent of different proportion, height
Molecularly Imprinted Polymer emulsion and inorganic active filler etc. have mixed a kind of many metal tripolyphosphates adhesive.This adhesive is due to body
It is that the dissolubility in water is less in the hydroxide corresponding to acidity and metal cation, it is possible to effectively cut off appearance
The path of the accumulation of salt in the surface soil, it is achieved the problem that sheet material occurs without anti-alkali in application process.
Detailed description of the invention
Embodiment 1:
A kind of many metal phosphates adhesive, is made up of the raw material of following weight portion: many metal phosphates colloid 40-60 part, goes
Ionized water 40-60 part, organosilicon moisture repellent 1-2 part, macromolecule emulsion 2-3 part, inorganic filler powder body 2-5 part.
Described many metal phosphates colloid includes aluminium hydroxide, II A family metal oxide, transition metal oxide, quality
Mark is phosphoric acid solution and the deionized water of 80%;Wherein, aluminium hydroxide, II A family metal oxide and transition metal oxide
Mol ratio be n1:n2:n3=(50-100): (0-50): (0-50), mass fraction be 80% phosphoric acid solution in institute's phosphoric acid
Molal quantity be: n4=3n1+2n2+2n3, the quality of deionized water is the 5%-20% of many metal phosphates colloid gross mass.
Described aluminium hydroxide is the powder body that purity is more than 95%.
Described II A family metal oxide is at least one in BeO, MgO, CaO, SrO and BaO, and purity is more than 98%, grain
Degree is less than 800 mesh.
Described II A family metal oxide is at least one in MgO and CaO.
Described transition metal oxide is FeO, CuO, ZnO, Cr2O3, MnO2And ZrO2In at least one, purity is more than
98%, granularity is less than 800 mesh.
Described organosilicon moisture repellent is methyl silicon sodium alcoholate, in isobutyl group sodium silanolate or isooctyltriethoxysilane
Kind.
Described macromolecule emulsion is styrene-acrylic emulsion, JS emulsion, the one in emulsified asphalt or modified acrylic acid emulsion.
Described inorganic filler powder body is at least one in white carbon, ultrafine kaolin and Ultra-fine Bentonite.
Concrete operation step is:
A. the preparation of many metal phosphates colloid: weigh aluminium hydroxide, II A family metal oxide and transition metal oxide, mixed
There-necked flask is put into after closing uniformly;Weighing phosphoric acid solution again, and be slowly added in there-necked flask by phosphoric acid solution, limit edged stirs
Mix;To there-necked flask reload temperature meter, agitator and reflux condensing tube respectively, then there-necked flask is put into the constant temperature of 80-100 DEG C
Heated and stirred in oil bath, question response system temperature stably starts timing later, adds deionized water stirring after reaction 20-40min
Uniformly;
B. the preparation of many metal phosphates adhesive: weigh many metal phosphates colloid, adds deionized water, adds and weigh
Organosilicon moisture repellent, macromolecule emulsion and inorganic filler powder body, in stirrer for mixing uniformly.
Embodiment 2:
A kind of many metal phosphates adhesive, is made up of the raw material of following weight portion: many metal phosphates colloid 40g, deionization
Water 40g, methyl silicon sodium alcoholate 1g, styrene-acrylic emulsion 2g, white carbon 2g.
Described many metal phosphates colloid includes that the raw material of following molar part is made: aluminium hydroxide n1=50mol, BeO n2
=1mol, FeO n3=1mol, mass fraction be 80% phosphoric acid solution in the molal quantity of institute's phosphoric acid be: n4=3n1+2n2+
2n3=154mol, also includes deionized water, and the quality of deionized water is the 15% of many metal phosphates colloid gross mass.
Described aluminium hydroxide is the powder body that purity is more than 95%.
The purity of BeO and FeO is more than 98%, and granularity is less than 800 mesh.
Concrete operation step is:
A. the preparation of many metal phosphates colloid: weigh aluminium hydroxide, BeO and FeO, puts into there-necked flask after mix homogeneously;
Weigh phosphoric acid solution again, and phosphoric acid solution is slowly added in there-necked flask, stirring while adding;Temperature is installed respectively additional to there-necked flask
Degree meter, agitator and reflux condensing tube, then there-necked flask is put into heated and stirred in the constant temperature oil bath of 90 DEG C, question response system temperature
Start timing after degree is stable, add deionized water after reaction 30min and stir;
B. the preparation of many metal phosphates adhesive: weigh many metal phosphates colloid, adds deionized water, adds and weigh
Organosilicon moisture repellent, macromolecule emulsion and inorganic filler powder body, in stirrer for mixing uniformly.
In embodiment 3-65, many metal phosphates adhesive and each process parameter are shown in Table 1-9, and wherein, aluminium hydroxide is
The purity powder body more than 95%, the purity of II A family metal oxide and transition metal oxide is more than 98%, and granularity is less than 800
Mesh, other are with embodiment 2.
In embodiment 17-65, organosilicon moisture repellent is methyl silicon sodium alcoholate, and macromolecule emulsion is styrene-acrylic emulsion, inorganic filler
Powder body is white carbon.
Many metal phosphates adhesive and each process parameter in table 1 embodiment 3-9
Many metal phosphates adhesive and each process parameter in table 2 embodiment 10-16
Many metal phosphates adhesive and each process parameter in table 3 embodiment 17-23
Many metal phosphates adhesive and each process parameter in table 4 embodiment 24-30
Many metal phosphates adhesive and each process parameter in table 5 embodiment 31-37
Many metal phosphates adhesive and each process parameter in table 6 embodiment 38-44
Many metal phosphates adhesive and each process parameter in table 7 embodiment 45-51
Many metal phosphates adhesive and each process parameter in table 8 embodiment 52-58
Many metal phosphates adhesive and each process parameter in table 9 embodiment 59-65
Embodiment 66:
A kind of expanded perlite thermal-nsulation plate using many metal tripolyphosphates adhesive to prepare, is made up of the raw material of following weight portion: swollen
Swollen perlite 40g, many metal phosphates adhesive 40g.
Described many metal phosphates adhesive is made up of the raw material of following weight portion: many metal phosphates colloid 40g, go from
Sub-water 40g, methyl silicon sodium alcoholate 1g, styrene-acrylic emulsion 2g, white carbon 2g.
Described many metal phosphates colloid includes that the raw material of following molar part is made: aluminium hydroxide n1=50mol, BeO n2
=1mol, FeO n3=1mol, mass fraction be 80% phosphoric acid solution in the molal quantity of institute's phosphoric acid be: n4=3n1+2n2+
2n3=154mol, also includes deionized water, and the quality of deionized water is the 15% of many metal phosphates colloid gross mass.
Described aluminium hydroxide is the powder body that purity is more than 95%.
The purity of BeO and FeO is more than 98%, and granularity is less than 800 mesh.
Concrete operation step is:
(1) preparation of many metal phosphates colloid: weigh aluminium hydroxide, BeO and FeO, puts into there-necked flask after mix homogeneously;
Weigh phosphoric acid solution again, and phosphoric acid solution is slowly added in there-necked flask, stirring while adding;Temperature is installed respectively additional to there-necked flask
Degree meter, agitator and reflux condensing tube, then there-necked flask is put into heated and stirred in the constant temperature oil bath of 90 DEG C, question response system temperature
Start timing after degree is stable, add deionized water after reaction 30min and stir;
(2) preparation of many metal phosphates adhesive: weigh many metal phosphates colloid, adds deionized water, adds weighing
Good organosilicon moisture repellent, macromolecule emulsion and inorganic filler powder body, in stirrer for mixing uniformly;
(3) weigh expanded perlite and many metal phosphates adhesive, many metal phosphates adhesive is poured into expanded perlite
In and stir;
(4) the hygral expansion perlite stirred is poured in the cuboid die cavity of electrically powered press, open electro-hydraulic press, with
The speed of 0.5mm/s at the uniform velocity presses, and compression ratio is 2;
(5) after the pressurize of 20s, demoulding process is carried out;
(6) wet expanded perlite thermal-nsulation plate uses microwave drier to be dried 10min under the dutycycle of 80%;
(7) expanded perlite thermal-nsulation plate, at ambient temperature natural cooling, the reality of expanded perlite thermal-nsulation plate performance test are taken out
Test and the results are shown in Table 10.
The physical property of table 10 expanded perlite thermal-nsulation plate
Relative to prior art, the present invention propose use phosphoric acid and poly-metal deoxide/hydroxide react prepare many
The method of metal phosphate colloid, and to based on this kind of colloid by add the organosilicon moisture repellent of different proportion, height
Molecularly Imprinted Polymer emulsion and inorganic active filler etc. have mixed a kind of many metal tripolyphosphates adhesive.This adhesive is due to body
It is that the dissolubility in water is less in the hydroxide corresponding to acidity and metal cation, it is possible to effectively cut off appearance
The path of the accumulation of salt in the surface soil, it is achieved the problem that sheet material occurs without anti-alkali in application process.
It should be noted that the weight portion unit in this patent can use g, kg etc..
Above-described is only the preferred embodiment of the present invention, it is noted that for a person skilled in the art,
Without departing under general idea premise of the present invention, it is also possible to making some changes and improvements, these also should be considered as the present invention's
Protection domain.
Claims (10)
1. metal phosphate adhesive more than a kind, it is characterised in that: it is made up of the raw material of following weight portion: many metal phosphates glue
Body 40-60 part, deionized water 40-60 part, organosilicon moisture repellent 1-2 part, macromolecule emulsion 2-3 part, inorganic filler powder body 2-5
Part.
Many metal phosphates adhesive the most according to claim 1, it is characterised in that: described many metal phosphates colloid bag
Include aluminium hydroxide, II A family metal oxide, transition metal oxide, mass fraction be 80% phosphoric acid solution and deionized water;
Wherein, the mol ratio of aluminium hydroxide, II A family metal oxide and transition metal oxide is n1:n2:n3=(50-100): (0-
50): (0-50), mass fraction be 80% phosphoric acid solution in the molal quantity of institute's phosphoric acid be: n4=3n1+2n2+2n3, deionized water
The 5%-20% that quality is many metal phosphates colloid gross mass.
Many metal phosphates adhesive the most according to claim 2, it is characterised in that: described aluminium hydroxide is that purity is more than
The powder body of 95%.
Many metal phosphates adhesive the most according to claim 2, it is characterised in that: described II A family metal oxide is
At least one in BeO, MgO, CaO, SrO and BaO, purity is more than 98%, and granularity is less than 800 mesh.
Many metal phosphates adhesive the most according to claim 4, it is characterised in that: described II A family metal oxide is
At least one in MgO and CaO.
Many metal phosphates adhesive the most according to claim 2, it is characterised in that: described transition metal oxide is
FeO, CuO, ZnO, Cr2O3, MnO2And ZrO2In at least one, purity be more than 98%, granularity be less than 800 mesh.
Many metal phosphates adhesive the most according to claim 1, it is characterised in that: described organosilicon moisture repellent is methyl
Sodium silanolate, the one in isobutyl group sodium silanolate or isooctyltriethoxysilane.
Many metal phosphates adhesive the most according to claim 1, it is characterised in that: described macromolecule emulsion is phenylpropyl alcohol breast
Liquid, JS emulsion, the one in emulsified asphalt or modified acrylic acid emulsion.
Many metal phosphates adhesive the most according to claim 1, it is characterised in that: described inorganic filler powder body is Linesless charcoal
At least one in black, ultrafine kaolin and Ultra-fine Bentonite.
The preparation method of many metal phosphates adhesive the most according to claim 1, it is characterised in that: concrete operations walk
Suddenly it is:
A. the preparation of many metal phosphates colloid: weigh aluminium hydroxide, II A family metal oxide and transition metal oxide, mixed
There-necked flask is put into after closing uniformly;Weighing phosphoric acid solution again, and be slowly added in there-necked flask by phosphoric acid solution, limit edged stirs
Mix;To there-necked flask reload temperature meter, agitator and reflux condensing tube respectively, then there-necked flask is put into the constant temperature of 80-100 DEG C
Heated and stirred in oil bath, question response system temperature stably starts timing later, adds deionized water stirring after reaction 20-40min
Uniformly;
B. the preparation of many metal phosphates adhesive: weigh many metal phosphates colloid, adds deionized water, adds weighing
Good organosilicon moisture repellent, macromolecule emulsion and inorganic filler powder body, in stirrer for mixing uniformly.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106833396A (en) * | 2017-03-23 | 2017-06-13 | 黑龙江省科学院石油化学研究院 | A kind of preparation method of low viscosity Phosphate adhesive |
CN108910856A (en) * | 2018-08-15 | 2018-11-30 | 济南大学 | The preparation method and products obtained therefrom of a kind of titanium phosphate containing calcium and the porous material of titanium hydrogen orthophosphate twin crystal phase |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102391792A (en) * | 2011-09-29 | 2012-03-28 | 哈尔滨工业大学 | Organic silicon resin/ phosphate composite adhesive and preparation method thereof |
CN105419652A (en) * | 2015-12-21 | 2016-03-23 | 哈尔滨船大森海技术开发有限公司 | Preparation method and curing method of flue gas turbine steam pressure chamber sealing material |
-
2016
- 2016-06-06 CN CN201610395445.3A patent/CN106047182A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102391792A (en) * | 2011-09-29 | 2012-03-28 | 哈尔滨工业大学 | Organic silicon resin/ phosphate composite adhesive and preparation method thereof |
CN105419652A (en) * | 2015-12-21 | 2016-03-23 | 哈尔滨船大森海技术开发有限公司 | Preparation method and curing method of flue gas turbine steam pressure chamber sealing material |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106833396A (en) * | 2017-03-23 | 2017-06-13 | 黑龙江省科学院石油化学研究院 | A kind of preparation method of low viscosity Phosphate adhesive |
CN108910856A (en) * | 2018-08-15 | 2018-11-30 | 济南大学 | The preparation method and products obtained therefrom of a kind of titanium phosphate containing calcium and the porous material of titanium hydrogen orthophosphate twin crystal phase |
CN108910856B (en) * | 2018-08-15 | 2021-10-26 | 济南大学 | Preparation method of porous material containing titanium calcium phosphate and titanium hydrogen phosphate double crystal phase and obtained product |
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