CN102277013B - Production method of active manganese dioxide for polysulfide sealant solidification - Google Patents
Production method of active manganese dioxide for polysulfide sealant solidification Download PDFInfo
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Abstract
The invention belongs to the technical field of inorganic materials, and relates to a production method of active manganese dioxide for the polysulfide sealant solidification. The production method provided by the invention comprises the following steps of: (1) fully mixing manganese dioxide and a fire retardant to obtain a mixture A; (2) fully mixing the mixture A with a coupling agent or a mixture of the coupling agent and a surfactant to obtain the active manganese dioxide. The production method provided by the invention is simple and safe, the reaction condition is mild, and the product obtained has advantages of high activity, aging resistance, deterioration resistance, convenient usage and the like.
Description
Technical field
The invention belongs to technical field of inorganic material, relate to a kind of production method of active manganese dioxide for polysulfide sealant solidification.
Background technology
The bi-component polysulfide seal gum with its excellent sealing property, is widely used in the fields such as aviation, building, traffic, waterproof.The chemical property of the mercaptan end group of liquid polysulphide rubber is more active, at normal temperatures can with many metal oxides, metal peroxides, inorganic oxidizer and organo-peroxide generation oxidizing reaction, thiol group generates disulfide linkage through oxidizing reaction, forms the rubber elastomer of high molecular.
At present, activated manganese dioxide is the solidifying agent of the most frequently used bi-component polysulfide seal gum.Manganse Dioxide is compared with plumbic oxide, and toxicity is low,, ultraviolet aging resistance stable with the seal gum of its preparation.The curing reaction of bi-component polysulfide seal gum is as follows:
2?~R?—?SH+MnO?
2?→?~?R?—?S?—?S?—?R?~?+MnO+H
2O
Adopt at present natural manganese ores through high-temperature roasting, with MnO
2Be reduced to Mn
2O
3, then add water slurrying, insert again in the disproportionation oxidizing reaction tank and (add in proportion sulfuric acid and NaClO
3, temperature is controlled at 90-96 ℃) react, make Mn
2O
3Change MnO into
2, then enter in the rinse bath and wash, add the bicarbonate of ammonia neutralization, washing, oven dry make manganese dioxide product.The product that this method is produced, MnO
2Content only has about 50%, poor stability, and activity is low during as the thiorubber solidifying agent, produces sometimes gases affect quality product and sealing effectiveness in the solidification process.This production technique is high to the grade requirement of manganese ore powder, can produce poisonous chlorine in the oxidizing reaction, adopts soda ash to absorb poor processing effect, and cost is large, and energy consumption is high, and is seriously polluted.Although the standby activated manganese dioxide technique of pure chemistry legal system is simple, the Manganse Dioxide activity is higher, but use procedure still exist the early stage rate of crosslinking fast, later stage solidifies slow, and the problems such as product degradation and use complex process, restricted to a certain extent the application and development of thiorubber and modified polysulfide rubber sealing prod.
Summary of the invention
The object of the present invention is to provide a kind of production method of active manganese dioxide for polysulfide sealant solidification, the prepared Manganse Dioxide of the method is active high.
The present invention is by the following technical solutions:
The production method of active manganese dioxide for polysulfide sealant solidification, comprise the steps: that (1) fully is mixed to get mixture A with Manganse Dioxide and fire retardant, (2) fully are mixed to get activated manganese dioxide with the mixture of mixture A and coupling agent or coupling agent and tensio-active agent.
Amount of flame-retardant agent is the 0.2-1.5wt% of Manganse Dioxide in the described step (1); The coupling agent consumption is the 0.3-3wt% of Manganse Dioxide in the described step (2), and described dosage of surfactant is the 1-3wt% of Manganse Dioxide, and mixing condition is at 80-125 ℃ of lower normal pressure ground and mixed 30-50min.
Described fire retardant is aluminium hydroxide, magnesium hydroxide, antimonous oxide or zinc phosphate.
Described coupling agent is silane coupling agent, titanate coupling agent, aluminate coupling agent or phosphate coupling agent.
Described silane coupling agent is: vinyltriethoxysilane, vinyltrimethoxy silane, the glycidyl allyl ether Trimethoxy silane, the n-propyl triethoxyl silane, the n-propyl Trimethoxy silane, the n-octyl triethoxyl silane, the n-octyl Trimethoxy silane, mercaptopropyl trimethoxysilane, mercaptopropyltriethoxysilane, 1,2 pairs of (trimethoxy is silica-based) ethane, 1,2 pair of (triethoxy is silica-based) ethane, the dodecyl Trimethoxy silane, γ-chloropropyl triethoxysilane, two (γ-(triethoxysilicane) propyl group) tetrasulfide, N-aminoethyl-γ-aminopropyltrimethoxysilane, N-aminoethyl-γ-aminopropyl triethoxysilane, the one or more kinds of combinations of γ-(methacryloxypropyl) propyl trimethoxy silicane; Described titanate coupling agent is sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three oleic acid acyloxy titanic acid ester, sec.-propyl three stearic acid acyloxy titanic acid ester, sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester, the complex compound of Di(dioctylpyrophosphato) ethylene titanate and trolamine, Di(dioctylpyrophosphato) ethylene titanate, tetra isopropyl (two octyloxy tetra-sodium ester groups) titanic acid ester, two (acetylacetone based) di-isopropyl titanic acid ester, the one or more kinds of combinations of two Triethanolamine di-isopropyl titanic acid ester; Described aluminate coupling agent is Ax-2 type aluminate coupling agent; Described phosphate coupling agent is the dioctyl phosphate coupling agent.
Described tensio-active agent is: ionogenic surfactant, nonionic surface active agent or amphoteric ionic surfactant.
Described ionogenic surfactant is oleic acid, potassium oleate, stearic acid, sodium stearate, potassium stearate, soft acid, soft acid sodium, soft acid potassium, tetradecanoic acid, Sodium tetradecanoate, potassium myristate, lauric acid, sodium laurate, potassium laurate, the succinate sodium sulfonate, the succinate potassium sulfonate, polyoxyethylene alkyl ether sulfate sodium, the sodium sulfovinate of 12-18 carbon unsaturated alcohol, the alpha-olefin sodium sulfonate, sodium laurylsulfonate, the alpha-sulfo monocarboxylate, petroleum sodium sulfonate, sodium lignosulfonate, the alpha-olefin potassium sulfonate, the alpha-sulfo monocarboxylate, mahogany acid potassium, lignosulfonic acid potassium, dodecyl trimethylammonium quaternary amine sodium or triethanol ammonium sodium; Described nonionic surface active agent is polyoxyethylene octylphenol ether, polyoxyethylene nonylphenol ether or Linolenic Acid enol Soxylat A 25-7; Described amphoteric ionic surfactant is Varion CDG-K, tridecyl dimethyl betaine, octodecyl betaine or sodium dodecyl aminopropionitrile.
The preparation process of described Manganse Dioxide is: with permanganate, manganous salt and alkaloid compound are to use water dissolution respectively in three containers after the ratio weighing of 1:1.5 ~ 2.2:2.10 ~ 4.65 in molar ratio, according to the first permanganate order of alkaloid compound behind the manganous salt again, control three's rate of feeding reacts than add for 1:1.5 ~ 2.2:2.10 ~ 4.65 and permanganate in advance, temperature of reaction is 40-100 ℃, system pH is 4-12, reaction times is 40 ~ 90min, then separating obtained solid is with 30-100 ℃ water washing, filter, be drying to obtain Manganse Dioxide.
Described permanganate is potassium permanganate, and manganous salt is manganous sulfate, and alkaloid compound is potassium hydroxide.
Production method of the present invention is simple, safety, reaction conditions is gentle, that products obtained therefrom has is active high, it is ageing-resistant to have, degeneration, the advantage such as easy to use, technological process is pollution-free, energy consumption is little, starting material convenient sources, byproduct of reaction recoverable, products obtained therefrom meets the thiorubber cross-linking properties fully, have the obvious long engineering time, short later stage solidification effect thoroughly solves thiorubber and stores degradation phenomena.Be particularly suitable for the solidifying agent of polysulfide sealant and modified polysulfide rubber, can also be used for other industrial circles, have broad application prospects.
Embodiment
Embodiment one
Take by weighing the potassium permanganate of 1180g, the manganous sulfate of 2265 g and the potassium hydroxide of 1120 g, be dissolved in respectively 60 ℃ hot water, after stirring fully dissolving, in 30.00 L reactors, react, according to the first permanganate order of alkaloid compound behind the manganous salt again, control three's rate of feeding reacts than add for 1:1.62:2.68 and permanganate in advance, the pH value is 5.8, temperature of reaction is 60 ℃, stirring reaction 40 min, then separating obtained solid obtains manganese dioxide product 1891g(and records MnO with 30 ℃ water washing, filtration, drying
2Content 85%, oil-absorption(number) 1.25 ml/g, pH 7.5, stacking volume 0.226 (g/ml), moisture content 2.1%, active phase 20-40 min); Above-mentioned manganese dioxide product is placed mixing machine, adding 6g aluminium hydroxide fully mixed 6 minutes, then add 25 g mercaptopropyltriethoxysilanes, carry out ground and mixed in 95 ℃ and process 10 min, add at last 30g succinate sodium sulfonate, obtain the 2034g activated manganese dioxide in 120 ℃ of mixed grinding 25 min.The product Fundamental Physical Properties is: outward appearance is the dark-brown powder, Manganse Dioxide content 80.5%, pH value 9.2, oil-absorption(number) 0.48 ml/g, moisture 2.6%, stacking volume 0.305 (g/ml), active phase 20-210 min.
Embodiment two
Take by weighing the potassium permanganate of 1180 g, the manganous sulfate of 2500kg and the potassium hydroxide of 1300g, be dissolved in respectively 70 ℃ hot water, after stirring fully dissolving, in 30.00 L reactors, react, according to the first permanganate order of alkaloid compound behind the manganous salt again, control three's rate of feeding reacts than add for 1:1.79:3.11 and permanganate in advance, the pH value is 8.8, temperature of reaction is 60 ℃, stirring reaction 50 min, then separating obtained solid is with 50 ℃ water washing, filtration, dry that 2050 g manganese dioxide products (record MnO
2Content 87%, oil-absorption(number) 1.15 ml/g, pH 9.25, stacking volume 0.276 (g/ml), moisture content 1.8%, active phase 15-40 min); 2050 g manganese dioxide products are placed mixing machine, add 8 g magnesium hydroxides and mix 8 min, then add 23 g sodium stearate and process the last 25 gAx-2 type aluminate coupling agents that add of mixing 8 min in 85 ℃, carry out ground and mixed in 110 ℃ and process 40 min, obtain the 2105g activated manganese dioxide.The product Fundamental Physical Properties is: outward appearance is the dark-brown powder, MnO
2Content 79.5%, pH value 9.8, oil-absorption(number) 0.425 ml/g, moisture 2.8%, stacking volume 0.315 (g/ml), active phase 20-210 min.
Embodiment three
Take by weighing the potassium permanganate of 1000g, the manganous sulfate of 2265g and the potassium hydroxide of 1035g, be dissolved in respectively 50 ℃ hot water, after stirring fully dissolving, in 30.00 L reactors, react, according to the first permanganate order of alkaloid compound behind the manganous salt again, control three's rate of feeding reacts than add for 1:1. 91:3.80 and permanganate in advance, the pH value is 10.1, temperature of reaction is 60 ℃, stirring reaction 75 min, then separating obtained solid with 80 ℃ water washing, filter, be drying to obtain manganese dioxide product 1880g(and record MnO
2Content 86%, oil-absorption(number) 1.05 ml/g, pH 9.45, stacking volume 0.256 (g/ml), moisture content 2.1%, active phase 20-40 min); Manganese dioxide product is placed mixing machine, add 10 g antimonous oxide combination treatment, 3 min, then add 30g n-octyl Trimethoxy silane, in 80 ℃ of combination treatment 5 min, add at last the 26g lauric acid and flood processing 30 min in 110 ℃ of environment of temperature, get the 2014g activated manganese dioxide.The product Fundamental Physical Properties is: outward appearance is the dark-brown powder, MnO
2Content 81.5%, pH value 10.35, oil-absorption(number) 0.435 ml/g, moisture 1.9%, stacking volume 0.325 (g/ml), active phase 20-210 min.
Embodiment four
Take by weighing the potassium permanganate of 1180g, the manganous sulfate of 2265g and the potassium hydroxide of 1600g, be dissolved in respectively 60 ℃ hot water, after stirring fully dissolving, in 30.00 L reactors, react, according to the first permanganate order of alkaloid compound behind the manganous salt again, control three's rate of feeding reacts than add for 1:1.62:2.68 and permanganate in advance, the pH value is 11.8, temperature of reaction is 60 ℃, stirring reaction 40 min, then separating obtained solid gets Manganse Dioxide 2008g(and records MnO with 100 ℃ water washing, filtration, drying
2Content 85%, oil-absorption(number) 1.25 ml/g, pH 10.5, stacking volume 0.286 (g/ml), moisture content 2.1%, active phase 20-40 min); The 2008g manganese dioxide product is placed mixing machine, add 8 g zinc phosphates and mix 6 min, then add 28g sec.-propyl three oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester and mix 5 min, add the 28g stearic acid at last and carry out ground and mixed at 125 ℃ and process 30 min in 90 ℃, get the 2071g activated manganese dioxide.The product Fundamental Physical Properties is: outward appearance is the dark-brown powder, Manganse Dioxide content 80.5%, pH value 10.2, oil-absorption(number) 0.48 ml/g, moisture 1.5%, stacking volume 0.305 (g/ml), active phase 20-300 min.
Get activated manganese dioxide 50 g that above-described embodiment 1,2,3,4 obtains, sulphur 1.2 g, dioctyl phthalate (DOP) 100 g, carbon black 10 g, vulkacit D 2 g, TMTD 1 g makes paste 1,2,3,4;
Replace embodiment 1 activated manganese dioxide with non-modified active Manganse Dioxide, make paste 5;
Replace embodiment 1 activated manganese dioxide with commercially available activated manganese dioxide, make paste 6;
Replace embodiment 1 activated manganese dioxide with the Honeywell activated manganese dioxide, make paste 7.
Get paste 1, put into the permanent chamber of constant temperature for 2,3,4,5,6, No. 7 and under 60 ℃ of environment, carry out the 0d-20d experiment of degenerating, respectively get 10 g after finishing and be cured experiment with commercially available bi-component polysulfide hollow sealing glue A component 100 g respectively, measure active phase and other performance perameters; Determination experiment the results are shown in Table 1.
Found out that by table 1 paste 1,2,3,4 ageing resistance are superior, little on its solidification effect impact after through 20 days degeneration, be conducive to the storage of product.
The basic curability contrast table of table 1
Annotate: stiffness units is Shao Shi A.Sense environmental conditions is 25 ± 2 ℃ of temperature, humidity 50%.
Claims (5)
1. the production method of active manganese dioxide for polysulfide sealant solidification, comprise the steps: that (1) is with permanganate, manganous salt and alkaloid compound are to use water dissolution respectively in three containers after the ratio weighing of 1:1.5 ~ 2.2:2.10 ~ 4.65 in molar ratio, according to the first permanganate order of alkaloid compound behind the manganous salt again, control three's rate of feeding reacts than add for 1:1.5 ~ 2.2:2.10 ~ 4.65 and permanganate in advance, temperature of reaction is 40-100 ℃, system pH is 4-12, reaction times is 40 ~ 90min, then separating obtained solid is with 30-100 ℃ water washing, filter, be drying to obtain Manganse Dioxide; Manganse Dioxide and fire retardant fully are mixed to get mixture A, and described fire retardant is aluminium hydroxide, magnesium hydroxide, antimonous oxide or zinc phosphate; (2) mixture with mixture A and coupling agent and tensio-active agent fully is mixed to get activated manganese dioxide, and described tensio-active agent is stearic acid, sodium stearate, lauric acid or succinate sodium sulfonate.
2. the production method of active manganese dioxide for polysulfide sealant solidification as claimed in claim 1 is characterized in that, amount of flame-retardant agent is the 0.2-1.5wt% of Manganse Dioxide in the described step (1); The coupling agent consumption is the 0.3-3wt% of Manganse Dioxide in the described step (2), and described dosage of surfactant is the 1-3wt% of Manganse Dioxide, and mixing condition is at 80-125 ℃ of lower normal pressure ground and mixed 30-50min.
3. the production method of active manganese dioxide for polysulfide sealant solidification as claimed in claim 2 is characterized in that, described coupling agent is silane coupling agent, titanate coupling agent, aluminate coupling agent or phosphate coupling agent.
4. the production method of active manganese dioxide for polysulfide sealant solidification as claimed in claim 3, it is characterized in that, described silane coupling agent is: vinyltriethoxysilane, vinyltrimethoxy silane, the glycidyl allyl ether Trimethoxy silane, the n-propyl triethoxyl silane, the n-propyl Trimethoxy silane, the n-octyl triethoxyl silane, the n-octyl Trimethoxy silane, mercaptopropyl trimethoxysilane, mercaptopropyltriethoxysilane, 1,2 pairs of (trimethoxy is silica-based) ethane, 1,2 pair of (triethoxy is silica-based) ethane, the dodecyl Trimethoxy silane, γ-chloropropyl triethoxysilane, two (γ-(triethoxysilicane) propyl group) tetrasulfide, N-aminoethyl-γ-aminopropyltrimethoxysilane, N-aminoethyl-γ-aminopropyl triethoxysilane, the one or more kinds of combinations of γ-(methacryloxypropyl) propyl trimethoxy silicane; Described titanate coupling agent is sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three oleic acid acyloxy titanic acid ester, sec.-propyl three stearic acid acyloxy titanic acid ester, sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester, the complex compound of Di(dioctylpyrophosphato) ethylene titanate and trolamine, Di(dioctylpyrophosphato) ethylene titanate, tetra isopropyl (two octyloxy tetra-sodium ester groups) titanic acid ester, two (acetylacetone based) di-isopropyl titanic acid ester, the one or more kinds of combinations of two Triethanolamine di-isopropyl titanic acid ester; Described aluminate coupling agent is Ax-2 type aluminate coupling agent; Described phosphate coupling agent is the dioctyl phosphate coupling agent.
5. the production method of active manganese dioxide for polysulfide sealant solidification as claimed in claim 1 is characterized in that, described permanganate is potassium permanganate, and manganous salt is manganous sulfate, and alkaloid compound is potassium hydroxide.
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| US10035926B2 (en) * | 2016-04-22 | 2018-07-31 | PRC—DeSoto International, Inc. | Ionic liquid catalysts in sulfur-containing polymer compositions |
| US10597468B2 (en) | 2017-07-20 | 2020-03-24 | The Boeing Company | Methods and compositions for curing a surface of an uncured polysulfide rubber |
| CN114057229B (en) * | 2020-08-03 | 2023-10-20 | 中国石油化工股份有限公司 | Activating agent and activating method of manganese dioxide solid slag |
| CN112480817B (en) * | 2020-11-26 | 2021-11-30 | 徐玲 | Heat-curable, moisture-curable or UV-curable corrosion-inhibiting composition |
| CN114316887B (en) * | 2022-01-07 | 2023-05-05 | 安徽大学 | Polysulfide sealant and preparation method thereof |
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Effective date of registration: 20210112 Address after: 450000 north section of West Fourth Ring Road, high tech Development Zone, Zhengzhou City, Henan Province Patentee after: Zhengzhou Yuchang building energy saving Technology Co.,Ltd. Address before: 450006 Xigang village, Lishui Town, Zhongyuan District, Henan, Zhengzhou Patentee before: ZHENGZHOU YUCHANG ORGANIC SILICON CHEMICAL INDUSTRY Co.,Ltd. |
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