CN102268227B - Inorganic solid binder with low melting point and preparation method thereof - Google Patents

Inorganic solid binder with low melting point and preparation method thereof Download PDF

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Publication number
CN102268227B
CN102268227B CN2011101492160A CN201110149216A CN102268227B CN 102268227 B CN102268227 B CN 102268227B CN 2011101492160 A CN2011101492160 A CN 2011101492160A CN 201110149216 A CN201110149216 A CN 201110149216A CN 102268227 B CN102268227 B CN 102268227B
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solution
equal
preparation
binding agent
inoganic solids
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Expired - Fee Related
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CN2011101492160A
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CN102268227A (en
Inventor
胡学芳
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JIANGMEN KEHENG INDUSTRY Co Ltd
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JIANGMEN KEHENG INDUSTRY Co Ltd
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Priority to CN2011101492160A priority Critical patent/CN102268227B/en
Priority to PCT/CN2011/082655 priority patent/WO2012163061A1/en
Publication of CN102268227A publication Critical patent/CN102268227A/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/24—Manufacture or joining of vessels, leading-in conductors or bases
    • H01J9/32—Sealing leading-in conductors
    • H01J9/323—Sealing leading-in conductors into a discharge lamp or a gas-filled discharge device
    • 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
    • C01B25/12—Oxides of phosphorus
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/02—Oxides or hydroxides
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J5/00—Details relating to vessels or to leading-in conductors common to two or more basic types of discharge tubes or lamps
    • H01J5/20—Seals between parts of vessels
    • H01J5/22—Vacuum-tight joints between parts of vessel
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J5/00—Details relating to vessels or to leading-in conductors common to two or more basic types of discharge tubes or lamps
    • H01J5/32—Seals for leading-in conductors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J61/00—Gas-discharge or vapour-discharge lamps
    • H01J61/02—Details
    • H01J61/30—Vessels; Containers
    • H01J61/35—Vessels; Containers provided with coatings on the walls thereof; Selection of materials for the coatings
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/24—Manufacture or joining of vessels, leading-in conductors or bases
    • H01J9/26—Sealing together parts of vessels
    • H01J9/265—Sealing together parts of vessels specially adapted for gas-discharge tubes or lamps
    • H01J9/266—Sealing together parts of vessels specially adapted for gas-discharge tubes or lamps specially adapted for gas-discharge lamps
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/40—Closing vessels
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases

Abstract

The invention discloses an inorganic solid binder and a preparation method thereof. The composition formula of the binder is as follows: nCaO.mBaO.xP2O5.yB2O3, wherein in the formula, n is larger than or equal to 0.8 and less than or equal to 1.1, m is more than or equal to 0.1 and less than or equal to 0.5, x is larger than or equal to 0.1 and less than or equal to 0.5, and y is larger than or equal to 0.3 and less than or equal to 1.0. The inorganic solid binder disclosed by the invention has fine particles and stable chemical property in suspension, starts to fuse at the temperature of about 300 DGE C, is completely fused at the temperature of 500+/-50 DEG C, takes a bonding effect, and is especially suitable for a temperature interval of 500-600 DEG C in a lamp craft bake tube manufacturing process. The preparation method is a chemical coprecipitation method which has a simple production process and is easy to industrialize.

Description

A kind of inorganic solid binder with low melting point and preparation method thereof
Technical field
The present invention relates to a kind of solid binder and preparation method thereof, particularly a kind of low-melting inoganic solids binding agent and preparation method thereof.
Background technology
The quality of luminescent lamp is determined by the performance quality of the control of the links of lamp manufacturing process and various starting material (comprising fluorescent material, electronic powder, tungsten filament etc.).The coating of fluorescent material is the important process process in the Fluorescent lamp production.
Binding agent is a chief component of phosphor suspension, and role is that fluorescent material is bonded on the glass-tube reliably.The composition and structure of binding agent how, affects the numerous characteristics of fluorescent coating, and for example fluorescent material is in clinging power on glass, the thoroughness of the thickness of coating, polymkeric substance thermolysis from coating etc.
In Fluorescent lamp production, water miscible binding agent can be divided into two large classes basically: a class is the modified-cellulose in the synthetic family macromolecule of water-soluble semi, such as carboxymethyl cellulose (CMC), methylcellulose gum (MC), hydroxypropylcellulose (HPC), Natvosol (HEC), hydroxy butyl methyl cellulose (HBMC) and Vltra tears (HPMC); Another kind of is polymer resin in the water-soluble synthetic family macromolecule, such as multipolymer and the polyoxyethylene (PEO) of multipolymer (PVM/MA), maleic anhydride and the iso-butylene (isobutylene) of polyacrylic acid (PAA), polymethyl acrylic acid (PMAA), poly-inclined to one side ammonium acrylate (APMA), maleic anhydride and polyvinyl methyl ethermaleic anhydride.
For the annular that also will carry out bending machining after the dusting and two D type lamp, the aluminum oxide that only adds ultra-fine grain diameter is inadequate, if not, the disadvantage of shedding and bisque cracking will occur in the knee of glass-tube, make the degraded appearance of fluorescent tube, light is logical to descend, and light decay rises.Therefore, for circular lamp and two D type lamps, except the alumina-reinforced agent of adding ultra-fine grain diameter, also to adopt to prevent that under the bend pipe service temperature fluorescent material from coming off and the glass powder with low melting point that ftractures is made nonvolatil strengthening agent.The amalgam ball sustains damage because rolling causes phosphor powder layer in transportation in the fluorescent tube bulb in order to prevent from being placed in, and part T5 luminescent lamp also adopts the glass powder with low melting point strengthening agent, and fluorescent material is sticked on the internal surface of glass-tube more securely.
Be necessary to develop a kind of novel ground, the inoganic solids binding agent that adhesive property is better.
Summary of the invention
The object of the present invention is to provide a kind of novel inoganic solids binding agent.
The technical solution used in the present invention is:
A kind of inoganic solids binding agent, its composition formula are nCaOmBaOxP 2O 5YB 2O 3, 0.8≤n in the formula≤1.1,0.1≤m≤0.5,0.1≤x≤0.5,0.3≤y≤1.0.
Preferably, its composition formula is nCaOmBaOxP 2O 5YB 2O 3, 0.95≤n in the formula≤1.0,0.2≤m≤0.4,0.3≤x≤0.5,0.6≤y≤0.8.
The preparation method of above-mentioned inoganic solids binding agent may further comprise the steps
1) raw material with calcic, barium or boron dissolves respectively, then is mixed to get solution A;
2) with phosphorous material dissolution, obtain solution B;
3) solution A is mixed with solution B, add ammoniacal liquor;
4) be heated to 80～90 ℃, stir, to generating white precipitate;
5) stirred 1～3 hour the pH to 7 of regulator solution～8;
6) with the white precipitate dehydration, the oven dry that obtain, 240～450 ℃ of calcinations;
7) with the fragmentation of calcination thing, washing, drying, obtain the inoganic solids binding agent.
Preferably, the raw material of calcic, barium or boron is water-soluble material, and the best is nitrocalcite, nitrate of baryta, boric acid.
Preferably, phosphorous raw material is water-soluble phosphate, and the best is (NH 4) 2HPO 4
Inoganic solids binding agent of the present invention, particle is thin, in suspension chemical stabilization, can about 300 ℃, begin melting, 500 ± 50 ℃ of complete meltings, play cohesive action, be specially adapted to 500～600 ℃ temperature range of lamp manufacturing process the baking process of lamp-tube.
Preparation method of the present invention, easy handling, the product homogeneity that obtains is good, reliable in quality.
Description of drawings
Fig. 1 is the DTA figure of inoganic solids binding agent of the present invention;
Fig. 2 is the TG figure of inoganic solids binding agent of the present invention.
Embodiment
A kind of inoganic solids binding agent, its composition formula are nCaOmBaOxP 2O 5YB 2O 3, 0.8≤n in the formula≤1.1,0.1≤m≤0.5,0.1≤x≤0.5,0.3≤y≤1.0.
Preferably, its composition formula is nCaOmBaOxP 2O 5YB 2O 3, 0.95≤n in the formula≤1.0,0.2≤m≤0.4,0.3≤x≤0.5,0.6≤y≤0.8.
The preparation method of above-mentioned inoganic solids binding agent may further comprise the steps
1) raw material with calcic, barium or boron dissolves respectively, then is mixed to get solution A;
2) with phosphorous material dissolution, obtain solution B;
3) solution A is mixed with solution B, add ammoniacal liquor;
4) be heated to 80～90 ℃, stir, to generating white precipitate;
5) stirred 1～3 hour the pH to 7 of regulator solution～8;
6) with the white precipitate dehydration, the oven dry that obtain, 240～450 ℃ of calcinations;
7) with the fragmentation of calcination thing, washing, drying, obtain the inoganic solids binding agent.
Preferably, the raw material of calcic, barium or boron is water-soluble material, and the best is nitrocalcite, nitrate of baryta, boric acid.
Preferably, phosphorous raw material is water-soluble phosphate, and the best is (NH 4) 2HPO 4
In the step 3), can react with solution A, B better for making ammoniacal liquor, generally when solution A, B mix, add ammoniacal liquor.
Step 4) is the homogeneity that guarantees to be heated, normal operation heating in water bath.Certainly, as long as can guarantee the homogeneity that solution is heated, also can use other type of heating.
In the preparation process, the purpose that adds ammoniacal liquor is to make the pH of solution to raise, and makes the raw material reaction precipitation in the solution, is to guarantee sufficient reacting, the addition of ammonia generally can raw material (raw material of calcic, barium, boron, phosphorus) total mole number 1.2～1.8 times.
The purpose of calcination is to make the precipitation melting, obtains the homogeneous molten mass, can select as required suitable calcination time, generally selects 3～4 hours.
Below in conjunction with embodiment, further specify the present invention.
Embodiment 1
CaO0.5BaO0.3P 2O 50.5B 2O 3Preparation
1) gets Ca (NO 3) 2.4H 2O 236.1 grams, Ba (NO 3) 2130.6 gram, H 3BO 364.9 gram is used respectively 1 L deionized water dissolving, is mixed to get solution A;
2) get (NH 4) 2HPO 483.1 gram is dissolved in the 1 L deionized water, obtains solution B;
3) solution A is mixed with solution B, add 0.1 L mass concentration and be 25% ammoniacal liquor;
4) be heated to 80 ℃, be stirred to and white precipitate occurs;
5) pH of regulator solution is 8, continues to stir 1 hour;
6) with the white precipitate dehydration, the oven dry that obtain, 250 ℃ of calcination 2h;
7) the calcination thing is crushed to required order number, washing, drying obtain the inoganic solids binding agent.
Fig. 1 is the DTA figure of embodiment 1 product; Fig. 2 is its TG figure, from Fig. 1, can find out that its initial melting temperature is 300 ℃ in 2.
Embodiment 2
1.1CaO0.2BaO0.25P 2O 50.6B 2O 3Preparation
1) gets Ca (NO 3) 2.4H 2O 259.7 grams, Ba (NO 3) 252.3 gram, H 3BO 377.9 gram is used respectively 1 L deionized water dissolving, is mixed to get solution A;
2) get (NH 4) 2HPO 469.3 gram is dissolved in the 1 L deionized water, obtains solution B;
3) solution A is mixed with solution B, add 0.1 L mass concentration and be 25% ammoniacal liquor;
4) be heated to 90 ℃, be stirred to and white precipitate occurs;
5) pH of regulator solution is 7.5, continues to stir 2 hours;
6) with the white precipitate dehydration, the oven dry that obtain, 350 ℃ of calcination 1.5h;
7) the calcination thing is crushed to required order number, washing, drying obtain the inoganic solids binding agent.
Embodiment 3
CaO0.4BaO0.35P 2O 50.7B 2O 3Preparation
1) gets Ca (NO 3) 2.4H 2O 236.1 grams, Ba (NO 3) 2104.5 gram, H 3BO 390.8 gram is used respectively 1 L deionized water dissolving, is mixed to get solution A;
2) get (NH 4) 2HPO 496.9 gram is dissolved in the 1 L deionized water, obtains solution B;
3) solution A is mixed with solution B, add 0.1 L mass concentration and be 25% ammoniacal liquor;
4) be heated to 85 ℃, be stirred to and white precipitate occurs;
5) pH of regulator solution is 7, continues to stir 3 hours;
6) with the white precipitate dehydration, the oven dry that obtain, 450 ℃ of calcination 0.5h;
7) the calcination thing is crushed to required order number, washing, drying obtain the inoganic solids binding agent.
Embodiment 4
0.8CaO0.1BaO0.4P 2O 50.8B 2O 3Preparation
1) takes by weighing nitrocalcite, nitrate of baryta, boric acid according to composition, obtain solution A with water dissolution;
2) take by weighing (NH 4) 2HPO 4Obtain solution B with water dissolution;
3) solution A is mixed with solution B, add capacity ammoniacal liquor;
4) be heated to 85 ℃, be stirred to and white precipitate occurs;
5) pH of regulator solution is 7, continues to stir 2.5 hours;
6) with the white precipitate dehydration, the oven dry that obtain, 250 ℃ of calcination 2h;
7) the calcination thing is crushed to required order number, washing, drying obtain the inoganic solids binding agent.
Embodiment 5
CaO0.3BaO0.5P 2O 5B 2O 3Preparation
1) takes by weighing nitrocalcite, nitrate of baryta, boric acid according to composition, obtain solution A with water dissolution;
2) take by weighing (NH 4) 2HPO 4Obtain solution B with water dissolution;
3) solution A is mixed with solution B, add capacity ammoniacal liquor;
4) be heated to 80 ℃, be stirred to and white precipitate occurs;
5) pH of regulator solution is 8, continues to stir 1 hour;
6) with the white precipitate dehydration, the oven dry that obtain, 300 ℃ of calcination 2h;
7) the calcination thing is crushed to required order number, washing, drying obtain the inoganic solids binding agent.
Embodiment 6
0.95CaO0.35BaO0.35P 2O 50.3B 2O 3Preparation
1) takes by weighing nitrocalcite, nitrate of baryta, boric acid according to composition, obtain solution A with water dissolution;
2) take by weighing (NH 4) 2HPO 4Obtain solution B with water dissolution;
3) solution A is mixed with solution B, add capacity ammoniacal liquor;
4) be heated to 87 ℃, be stirred to and white precipitate occurs;
5) pH of regulator solution is 8, continues to stir 1 hour;
6) with the white precipitate dehydration, the oven dry that obtain, 200 ℃ of calcination 3h;
7) the calcination thing is crushed to required order number, washing, drying obtain the inoganic solids binding agent.
Inoganic solids binding agent of the present invention, particle is thin, in suspension chemical stabilization, can about 300 ℃, begin melting, 500 ± 50 ℃ of complete meltings, play cohesive action, be specially adapted to 500～600 ℃ temperature range of lamp manufacturing process the baking process of lamp-tube.
Preparation method of the present invention, easy handling, the product homogeneity that obtains is good, reliable in quality.

Claims (3)

1. inoganic solids binding agent, its composition formula is nCaOmBaOxP 2O 5YB 2O 3, 0.8≤n in the formula≤1.1,0.1≤m≤0.5,0.1≤x≤0.5,0.3≤y≤1.0.
2. a kind of inoganic solids binding agent according to claim 1, its composition formula is nCaOmBaOxP 2O 5YB 2O 3, 0.95≤n in the formula≤1.0,0.2≤m≤0.4,0.3≤x≤0.5,0.6≤y≤0.8.
3. the preparation method of claim 1 or 2 described inoganic solids binding agents may further comprise the steps
1) raw material with calcic, barium or boron dissolves respectively, then is mixed to get solution A;
2) with phosphorous material dissolution, obtain solution B;
3) solution A is mixed with solution B, add ammoniacal liquor;
4) be heated to 80～90 ℃, stir, to generating white precipitate;
5) stirred 1～3 hour the pH to 7 of regulator solution～8;
6) with the white precipitate dehydration, the oven dry that obtain, 240～450 ℃ of calcinations;
7) with the fragmentation of calcination thing, washing, drying, obtain the inoganic solids binding agent;
Wherein, the raw material of calcic, barium or boron is nitrocalcite, nitrate of baryta, boric acid, and phosphorous raw material is (NH 4) 2HPO 4
CN2011101492160A 2011-06-03 2011-06-03 Inorganic solid binder with low melting point and preparation method thereof Expired - Fee Related CN102268227B (en)

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PCT/CN2011/082655 WO2012163061A1 (en) 2011-06-03 2011-11-23 Low melting point inorganic solid binder and preparation process thereof

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1860203A (en) * 2003-10-21 2006-11-08 住友化学株式会社 Fluorescent material and fluorescent material paste

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS554152B2 (en) * 1973-07-25 1980-01-29
JPH09249854A (en) * 1996-03-14 1997-09-22 Shin Etsu Chem Co Ltd Low-melting point glass adhesive and bonding
JP2002145649A (en) * 2000-11-07 2002-05-22 Asahi Fiber Glass Co Ltd Method for producing hardenable inorganic composition
US20040178734A1 (en) * 2003-03-13 2004-09-16 Yoshihisa Nagasaki Fluorescent device, fluorescent lamp and glass composite
KR20100003861A (en) * 2008-07-02 2010-01-12 희성전자 주식회사 Binding agent for fixing fluorescent material at low temperature firing

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1860203A (en) * 2003-10-21 2006-11-08 住友化学株式会社 Fluorescent material and fluorescent material paste

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