CN105924666A - Efficient foaming agent and preparation method thereof - Google Patents
Efficient foaming agent and preparation method thereof Download PDFInfo
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- CN105924666A CN105924666A CN201610237584.3A CN201610237584A CN105924666A CN 105924666 A CN105924666 A CN 105924666A CN 201610237584 A CN201610237584 A CN 201610237584A CN 105924666 A CN105924666 A CN 105924666A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/104—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/18—Binary blends of expanding agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2300/00—Characterised by the use of unspecified polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/329—Phosphorus containing acids
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention discloses an efficient foaming agent and a preparation method thereof. According to the preparation method, thionine is added into the raw materials, polythionine is deposited on the surface of the foaming agent, and thus the resistance of the foaming agent is effectively improved. In step (1), a mixed solution is prepared in a water bath with a constant temperature of 70 DEG C so as to guarantee that hydrazine hydrate can form a stable solution and the dissolution speed is accelerated, the pH of the mixed solution in the step (1) is 5.0, and under the acidity hydrazine hydrate can carry out condensation reaction most easily. In the step (2), a biurea intermediate is prepared by an infrared microwave method, and compared with the conventional hydrothermal method, the reaction speed is accelerated. In the step (4), a three electrode system is adopted in the electrified system, the work electrode is a glass-carbon electrode, the counter electrode is a platinum electrode, the reference electrode is an Ag/AgCl electrode, and compared with the two electrode system, a more stable and constant voltage is provided. In the step (5), the organic solvent is a propylene glycol solution, which can effectively remove impurities in the foaming agent.
Description
Technical field
The invention belongs to chemical field, particularly to a kind of efficient aerating powder and preparation method thereof.
Background technology
Plastic foamed technology origin is remote.It is the foam bakelite at the initial stage twenties the earliest, produces by the similar method manufacturing foam rubber；Hard polyurethane foams and polystyrene foam occur the thirties；There are polyethylene, polyvinyl chloride, epoxy resin, phenol formaldehyde foam the forties；Then there are expandable polystyrene foam and flexible polyurethane foams the fifties.Essentially all of plastics, including thermoplasticity with heat cured can foam as foamed plastics.As: the invention discloses a kind of PVC foamed plastics foaming agent, be made up of the raw material of following weight portion: azodicarbonamide potassium formate 8-12 part, p-toluene sulfonylsemicarbazide 4-6 part, to (N-methoxymethylamide base) benzene sulfonyl hydrazide 2-5 part, sodium sulfate of polyethenoxy ether of fatty alcohol 1-2 part, ammonium carbonate 2-4 part, monoethanolamine 2-3 part, urea 1-3 part, lead stearate 0.5-0.8 part, benzoic acid 3-6 part, calcium oxide 2-4 part, propane diols 15-20 part.For another example: the present invention relates to the preparation method of the foaming agent of a kind of high dispersive, main method: the present invention uses simply dissolving-adsorption precipitation method to select natural minerals montmorillonite to make blowing agent activator, so that foaming agent does not lumps, reunites.The foaming agent always performance based on foaming agent itself of these inventions improves, and the most more contributes for this well of performance of foamed plastics for foaming agent.
Summary of the invention
Problem to be solved by this invention is to provide a kind of efficient aerating powder and preparation method thereof.
To achieve these goals, the technical scheme that the present invention takes is:
A kind of efficient aerating powder, its raw material includes: hydrazine hydrate 8-12 part, urea 3-5 part, dihydric phosphate 2-3 part, phosphatase 11-2 parts and sulphur a beautiful gem 2-3 part.
A kind of efficient aerating powder preparation method, comprises the steps:
(1) urea is dissolved in hydrazine hydrate, then dihydric phosphate is dissolved wherein, by adding phosphoric acid in solution, the pH value of solution is transferred to 4.5-6.5；
(2) from 195 DEG C, the mixed solution of hydrazine hydrate being warming up to 215 DEG C, 30-60 minute heating-up time, maintain thermotonus 1.5-8 hour under 200-245 DEG C of temperature conditions, condensation generates biruea intermediate；
(3) the biruea intermediate that step (2) generates, under aerobic condition, is heated to 260-300 DEG C, reacts 0.5-2 hour, and biruea intermediate oxidation obtains foaming agent crude product；
(4) foaming agent crude product is mixed with sulphur a beautiful gem, dissolve in the secondary aqueous solution, solution is carried out energising process, using cyclic voltammetry that sulphur a beautiful gem is deposited on foaming agent crude product surface, voltage is-5～5v, sweeps speed for 0.1-0.5v/s, scanning 30-50 circle, can complete the deposition of sulphur a beautiful gem；
(5) step (4) prepares foaming agent crude product to clean in organic solution 3-7 time, then use distilled water to clean 3-5 time, dry at 45-60 DEG C, foaming agent i.e..
Preferably, in described step (1), mixed solution uses constant temperature water bath 70 DEG C preparation.
Preferably, in described step (1), the pH of mixed solution is 5.0.
Preferably, in described (2), the preparation method of biruea intermediate uses method prepared by infrared microwave.
Preferably, the three-electrode system that the electrifying system of described step (4) uses, working electrode is glass-carbon electrode, is platinum electrode to electrode, and reference electrode is Ag/AgCl electrode.
Preferably, the organic solvent of described step (5) is propylene glycol solution.
nullBeneficial effect: the invention provides a kind of efficient aerating powder and preparation method thereof，Interpolation sulphur a beautiful gem in its raw material，This material occurs polymerisation to produce netted polysulfide a beautiful gem in the case of energising，Polysulfide a beautiful gem is deposited on the surface of foaming agent can effectively improve the resistance of foaming agent，In described step (1), mixed solution uses constant temperature water bath 70 DEG C preparation，This method ensure that hydrazine hydrate forms stable solution，And accelerate the speed dissolved，In described step (1), the pH of mixed solution is 5.0，Under this acidity, hydrazine hydrate is easiest to condensation reaction，In described (2), the preparation method of biruea intermediate uses method prepared by infrared microwave，This method can add the speed of fast response compared to traditional hydro-thermal method，The three-electrode system that the electrifying system of described step (4) uses，Working electrode is glass-carbon electrode，It is platinum electrode to electrode，Reference electrode is Ag/AgCl electrode，This three-electrode system can provide compared to two electrode systems stablizes constant voltage，The organic solvent of described step (5) is propylene glycol solution，Propylene glycol solution can effectively remove the impurity in foaming agent.
Detailed description of the invention
Embodiment 1:
A kind of efficient aerating powder, its raw material includes: hydrazine hydrate 8 parts, 3 parts of urea, dihydric phosphate 2 parts, phosphatase 11 part and sulphur a beautiful gem 2 parts.
Its processing technology comprises the steps:
(1) being dissolved in hydrazine hydrate by urea, then dissolved wherein by dihydric phosphate, mixed solution uses constant temperature water bath 70 DEG C preparation, by adding phosphoric acid in solution, the pH value of solution is transferred to 5.0；
(2) method using infrared microwave to prepare, is warming up to 215 DEG C by the mixed solution of hydrazine hydrate from 195 DEG C, 30 minutes heating-up times, maintains thermotonus 1.5 hours under 200 DEG C of temperature conditionss, and condensation generates biruea intermediate；
(3) the biruea intermediate that step (2) generates, under aerobic condition, is heated to 260 DEG C, reacts 0.5 hour, and biruea intermediate oxidation obtains foaming agent crude product；
(4) foaming agent crude product is mixed with sulphur a beautiful gem, the secondary aqueous solution dissolves, solution is carried out energising process, the three-electrode system that electrifying system uses, working electrode is glass-carbon electrode, being platinum electrode to electrode, reference electrode is Ag/AgCl electrode, uses cyclic voltammetry that sulphur a beautiful gem is deposited on foaming agent crude product surface, voltage is-5～5v, sweeping speed is 0.1v/s, scanning 30 circle, can complete the deposition of sulphur a beautiful gem；
(5) step (4) prepares foaming agent crude product to clean in propane diols liquid 3 times, then use distilled water to clean 3 times, dry at 45 DEG C, foaming agent i.e..
Embodiment 2:
A kind of efficient aerating powder, its raw material includes: hydrazine hydrate 10 parts, 5 parts of urea, dihydric phosphate 3 parts, phosphoric acid 2 parts and sulphur a beautiful gem 3 parts.
Its processing technology comprises the steps:
(1) being dissolved in hydrazine hydrate by urea, then dissolved wherein by dihydric phosphate, mixed solution uses constant temperature water bath 70 DEG C preparation, by adding phosphoric acid in solution, the pH value of solution is transferred to 5.0；
(2) method using infrared microwave to prepare, is warming up to 215 DEG C by the mixed solution of hydrazine hydrate from 195 DEG C, 45 minutes heating-up times, maintains thermotonus 2.5 hours under 220 DEG C of temperature conditionss, and condensation generates biruea intermediate；
(3) the biruea intermediate that step (2) generates, under aerobic condition, is heated to 280 DEG C, reacts 1 hour, and biruea intermediate oxidation obtains foaming agent crude product；
(4) foaming agent crude product is mixed with sulphur a beautiful gem, the secondary aqueous solution dissolves, solution is carried out energising process, the three-electrode system that electrifying system uses, working electrode is glass-carbon electrode, being platinum electrode to electrode, reference electrode is Ag/AgCl electrode, uses cyclic voltammetry that sulphur a beautiful gem is deposited on foaming agent crude product surface, voltage is-5～5v, sweeping speed is 0.25v/s, scanning 45 circle, can complete the deposition of sulphur a beautiful gem；
(5) step (4) prepares foaming agent crude product to clean in propane diols liquid 4 times, then use distilled water to clean 3 times, dry at 55 DEG C, foaming agent i.e..
Embodiment 3:
A kind of efficient aerating powder, its raw material includes: hydrazine hydrate 12 parts, 5 parts of urea, dihydric phosphate 3 parts, phosphoric acid 2 parts and sulphur a beautiful gem 3 parts.
Its processing technology comprises the steps:
(1) being dissolved in hydrazine hydrate by urea, then dissolved wherein by dihydric phosphate, mixed solution uses constant temperature water bath 70 DEG C preparation, by adding phosphoric acid in solution, the pH value of solution is transferred to 5.0；
(2) method using infrared microwave to prepare, is warming up to 215 DEG C by the mixed solution of hydrazine hydrate from 195 DEG C, 60 minutes heating-up times, maintains thermotonus 4 hours under 245 DEG C of temperature conditionss, and condensation generates biruea intermediate；
(3) the biruea intermediate that step (2) generates, under aerobic condition, is heated to 300 DEG C, reacts 2 hours, and biruea intermediate oxidation obtains foaming agent crude product；
(4) foaming agent crude product is mixed with sulphur a beautiful gem, the secondary aqueous solution dissolves, solution is carried out energising process, the three-electrode system that electrifying system uses, working electrode is glass-carbon electrode, being platinum electrode to electrode, reference electrode is Ag/AgCl electrode, uses cyclic voltammetry that sulphur a beautiful gem is deposited on foaming agent crude product surface, voltage is-5～5v, sweeping speed is 0.5v/s, scanning 50 circle, can complete the deposition of sulphur a beautiful gem；
(5) step (4) prepares foaming agent crude product to clean in propane diols liquid 7 times, then use distilled water to clean 5 times, dry at 60 DEG C, foaming agent i.e..
After process above, taking out sample respectively, measurement result is as follows:
Can draw according to above table data, when embodiment 2 parameter, the consummate degree of foaming agent after preparation is 99.99%, production cycle is 4.5h, produce the foaming dosage 23g that 1kg plastics need, contribution rate to foamed plastics resistance is 22%, and prior art standard is consummate degree is 99.95%, production cycle is 7h, produce the foaming dosage 30g that 1kg plastics need, contribution rate to foamed plastics resistance is 5%, this shows that the foaming agent purity of the present invention is high, with short production cycle, gas release is big, the resistance of foamed plastics can be effectively improved, so the present invention has significant superiority.
nullThe invention provides a kind of foaming agent and preparation method thereof，Interpolation sulphur a beautiful gem in its raw material，This material occurs polymerisation to produce netted polysulfide a beautiful gem in the case of energising，Polysulfide a beautiful gem is deposited on the surface of foaming agent can effectively improve the resistance of foaming agent，In described step (1), mixed solution uses constant temperature water bath 70 DEG C preparation，This method ensure that hydrazine hydrate forms stable solution，And accelerate the speed dissolved，In described step (1), the pH of mixed solution is 5.0，Under this acidity, hydrazine hydrate is easiest to condensation reaction，In described (2), the preparation method of biruea intermediate uses method prepared by infrared microwave，This method can add the speed of fast response compared to traditional hydro-thermal method，The three-electrode system that the electrifying system of described step (4) uses，Working electrode is glass-carbon electrode，It is platinum electrode to electrode，Reference electrode is Ag/AgCl electrode，This three-electrode system can provide compared to two electrode systems stablizes constant voltage，The organic solvent of described step (5) is propylene glycol solution，Propylene glycol solution can effectively remove the impurity in foaming agent.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every equivalent structure utilizing description of the invention content to be made or equivalence flow process conversion; or directly or indirectly it is used in other relevant technical fields, the most in like manner it is included in the scope of patent protection of the present invention.
Claims (8)
1. an efficient aerating powder, it is characterised in that its raw material includes: hydrazine hydrate 8-12 part,
Urea 3-5 part, dihydric phosphate 2-3 part, phosphatase 11-2 parts.
A kind of efficient aerating powder the most according to claim 1, it is characterised in that it is former
Material is also added with sulphur a beautiful gem 2-3 part.
3. the method for the efficient aerating powder prepared described in claim 1, it is characterised in that:
Comprise the steps:
(1) urea is dissolved in hydrazine hydrate, then dihydric phosphate is dissolved wherein, logical
Cross interpolation phosphoric acid in solution, the pH value of solution is transferred to 4.5-6.5；
(2) mixed solution of hydrazine hydrate is warming up to 215 DEG C from 195 DEG C, heating-up time 30-60
Minute, under 200-245 DEG C of temperature conditions, maintaining thermotonus 1.5-8 hour, condensation generates
Biruea intermediate；
(3) the biruea intermediate that step (2) generates, under aerobic condition, is heated to
260-300 DEG C, reacting 0.5-2 hour, it is thick that biruea intermediate oxidation obtains efficient aerating powder
Product；
(4) foaming agent crude product is mixed with sulphur a beautiful gem, dissolve in the secondary aqueous solution, to solution
Carry out energising process, use cyclic voltammetry that sulphur a beautiful gem is deposited on foaming agent crude product surface, voltage
For-5～5v, sweeping speed is 0.1-0.5v/s, and scanning 30-50 circle can complete the heavy of sulphur a beautiful gem
Long-pending；
(5) prepared for step (4) foaming agent crude product is cleaned in organic solution 3-7 time, so
Rear use distilled water cleans 3-5 time, dries, foaming agent i.e. at 45-60 DEG C.
4., according to a kind of efficient aerating powder preparation method described in claim 3, its feature exists
In: in described step (1), mixed solution uses constant temperature water bath 70 DEG C preparation.
5., according to a kind of efficient aerating powder preparation method described in claim 3, its feature exists
In: in described step (1), the pH of mixed solution is 5.0.
6., according to a kind of efficient aerating powder preparation method described in claim 3, its feature exists
In: in described step (2), the preparation method of biruea intermediate uses infrared microwave to prepare
Method.
7., according to a kind of efficient aerating powder preparation method described in claim 3, its feature exists
In: the three-electrode system that the electrifying system of described step (4) uses, working electrode is glass carbon
Electrode, is platinum electrode to electrode, and reference electrode is Ag/AgCl electrode.
8., according to a kind of efficient aerating powder preparation method described in claim 3, its feature exists
In: the organic solvent of step (5) is propylene glycol solution.
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| CN201610237584.3A CN105924666A (en) | 2016-04-15 | 2016-04-15 | Efficient foaming agent and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1986524A (en) * | 2006-12-21 | 2007-06-27 | 巨化集团技术中心 | Preparing process for biurea |
| CN104892463A (en) * | 2015-04-16 | 2015-09-09 | 杭州海虹精细化工有限公司 | Process for producing biurea through optimized urea method |
| CN105440476A (en) * | 2015-11-29 | 2016-03-30 | 惠州卫生职业技术学院 | Preparation method of plastic film |
-
2016
- 2016-04-15 CN CN201610237584.3A patent/CN105924666A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1986524A (en) * | 2006-12-21 | 2007-06-27 | 巨化集团技术中心 | Preparing process for biurea |
| CN104892463A (en) * | 2015-04-16 | 2015-09-09 | 杭州海虹精细化工有限公司 | Process for producing biurea through optimized urea method |
| CN105440476A (en) * | 2015-11-29 | 2016-03-30 | 惠州卫生职业技术学院 | Preparation method of plastic film |
Non-Patent Citations (3)
| Title |
|---|
| 严瑞瑄主编: "《水处理剂应用手册》", 30 June 2003 * |
| 全造纸标准化中心编: "《造纸工业用化工材料手册》", 31 December 1998 * |
| 韩长日，宋小平主编: "《精细有机化工产品生产技术手册 下》", 30 June 2010 * |
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Application publication date: 20160907 |