CN108395833A - A kind of preparation method of freeze proof melt type watertight interface agent - Google Patents
A kind of preparation method of freeze proof melt type watertight interface agent Download PDFInfo
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- CN108395833A CN108395833A CN201810137605.3A CN201810137605A CN108395833A CN 108395833 A CN108395833 A CN 108395833A CN 201810137605 A CN201810137605 A CN 201810137605A CN 108395833 A CN108395833 A CN 108395833A
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Abstract
The present invention relates to construction material preparing technical fields, and in particular to a kind of preparation method of freeze proof melt type watertight interface agent.The present invention is to make polyurethane acrylate prepolymer by oneself as base material, from preparing silicon collosol and shaping phase-change material as accelerating agent, and it is aided with coconut oil and ammonium carbonate etc. and freeze proof melt type watertight interface agent is prepared, pass through polycaprolactone glycol decompression dehydration first, it adds hydroxy-ethyl acrylate and hydroquinone reaction generates line style self-control polyurethane acrylate prepolymer, lauryl sodium sulfate is recycled to be modified the nano silicon dioxide of water resistance, make nano silicon dioxide uniform adsorption in substrate surface, white carbon and the tetradecane are mixed, so that the tetradecane is adsorbed on white carbon surface, continue to add coconut oil, aliphatic acid in coconut oil is adsorbed at the active site of base material, prevent freeze thawing from further occurring, in addition ammonium carbonate is added into base material, further functioning as prevents from freezing, melt the effect of ice and snow, it is with a wide range of applications.
Description
Technical field
The present invention relates to construction material preparing technical fields, and in particular to a kind of preparation side of freeze proof melt type watertight interface agent
Method.
Background technology
Building is before decoration, and often there are many fine cracks and pores for surface of wall.In a humidity environment, water
And it includes salt branch infiltrate through inside concrete along fine cracks and pore, corroded internal reinforcing bar, made its life
Rust and expansion, have seriously affected the service life of building.In order to solve these problems, many producers can apply before construction to wall
Last layer interfacial agents enhance its surface strength.
Interfacial agents are a kind of adhesive, have superpower bonding force, excellent water resistance, resistance to ag(e)ing.Improve plastering sand
Starch to the adhesion strength of base, can effectively avoid coat of plaster hollowing, fall off, shrinkage cracking the problems such as.For handling concrete, adding
The surfaces such as gas concrete, Dinas brickes and flyash brick are solved since these water absorbent surfaces are strong or smooth cause interface not easy to stick
It connects, causes coat of plaster hollowing, cracking, peeling etc..It can greatly enhance between new-old concrete and concrete and plastering mortar
Cohesive force.The dabbing process on conventional concrete surface can be replaced, improve air entrained concrete surface plastering technique, be to build in the modern times
It builds and the indispensable supplementary material of decoration construction.
However, traditional interface agent on the market, only forms a tunic in surface of wall, can not penetrate into inside wall,
It is combined with concrete.In addition, some disadvantages of traditional interfacial agents also generally existing, such as:1, poor water resistance, especially intolerant to boiling
Water, it is easy to moisture absorption, it easily comes unglued in wet environment;2, durability is poor;3, poor heat resistance, the glue-line after solidification has thermoplasticity, soft
It is low to change point(40~80 DEG C), as temperature increases, intensity drastically declines, and creep easily occurs, it is impossible to be used in temperature compared with
High occasion uses;4, freeze-thaw resistance is poor, -5 DEG C or less easy freezings, generates demulsifying phenomenon;5, with the bonding of Conventional insulation
Performance is poor, easily it is cracking, fall off, hollowing phenomena such as;6, traditional interface agent is often used some containing harmful substances such as formaldehyde
Raw material, threaten the health of user.
Therefore, a kind of interfacial agents that can solve above-mentioned performance issue are developed to have important practical significance.
Invention content
The technical problems to be solved by the invention:For current traditional interface agent, that there are freeze-thaw resistances is poor, temperature less than-
Easy freezing at 5 DEG C, generate demulsifying phenomenon, while there is also adhesive property difference and poor water resistance, easily it is cracking, fall off, moisture absorption
Phenomena such as, it can not meet the defect of market demands, provide a kind of preparation method of freeze proof melt type watertight interface agent.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of preparation method of freeze proof melt type watertight interface agent, it is characterised in that specifically preparation process is:
(1)It weighs 50~60mL polycaprolactone glycols and is added in the four-hole boiling flask equipped with blender, thermometer and condenser pipe and stir
It mixes, after stirring, and decompression dehydration, stirring thing is obtained, is continued stirring thing, hydroxy-ethyl acrylate, hydroquinone and dioxygen
Water mixing, which is placed in beaker, to be stirred to react, and cooling discharging obtains self-control polyurethane acrylate prepolymer;
(2)Deionized water, ethyl orthosilicate and absolute ethyl alcohol are mixed and is placed in beaker and stirs, obtains stirring liquid, then to beaker
The middle hydrochloric acid that agitated liquid product 0.5% is added dropwise, continues to keep the temperature hybrid reaction, reaction solution is obtained, by reaction solution and dodecyl sulphate
Sodium, which mixes, is put into ultrasonic disperse in ultrasonic wave separating apparatus, still aging after ultrasonic disperse, and discharging is obtained from preparing silicon collosol;
(3)White carbon and the tetradecane are mixed to be placed in vacuum pump by equal mass ratioes and reacted so that the tetradecane is adsorbed on white carbon
Surface, grinding discharging, obtains shaping phase-change material powder;
(4)It counts in parts by weight, it is molten to weigh 35~45 parts of self-control polyurethane acrylate prepolymers, 12~16 parts of self-control silicon respectively
Glue, 6~8 parts of shaping phase-change materials and the mixing of 24~32 parts of deionized waters are placed in blender and stir, then add 2~4 parts it is anhydrous
Ethyl alcohol, 1~3 part of silicone emulsion, 3~5 portions of coconut oil and 2~4 parts of ammonium carbonates, continue to be mixed, cooling discharging is to get freeze proof
Melt type watertight interface agent.
Step(1)The whipping temp is 95~100 DEG C, and mixing time is 12~16min, and decompression dehydration pressure is
0.06~0.08Mpa, decompression dehydration time are 21~25min, stirring thing, hydroxy-ethyl acrylate, hydroquinone and mass fraction
Mass ratio for 26% hydrogen peroxide is 5:2:2:1, it is 53~64 DEG C to be stirred to react temperature, and it is 1~2h to be stirred to react the time.
Step(2)The volume ratio of the deionized water, ethyl orthosilicate and absolute ethyl alcohol is 2:4:1, whipping temp is
50~52 DEG C, mixing time is 12~16min, and the mass fraction of hydrochloric acid is 24%, and the reaction was continued, and the time is 21~27min, reaction
Liquid and the mass ratio of lauryl sodium sulfate are 4:1, ultrasonic disperse frequency be 24~32kHz, the ultrasonic disperse time be 35~
45min, still aging time are 1~2 day.
Step(3)The reaction pressure is 0.06~0.08Mpa, and the reaction time is 16~20min.
Step(4)The whipping temp is 45~55 DEG C, and mixing time is 35~45min, and it is 75 to continue whipping temp
~85 DEG C, continuation mixing time is 1~2h.
Compared with other methods, advantageous effects are the present invention:
(1)The present invention is to make polyurethane acrylate prepolymer by oneself as base material, from preparing silicon collosol and shaping phase-change material as rush
Into agent, and it is aided with coconut oil and ammonium carbonate etc. and freeze proof melt type watertight interface agent is prepared, is subtracted first by polycaprolactone glycol
Press-dehydrating adds hydroxy-ethyl acrylate and hydroquinone after dehydration, and polymerisation occurs under catalytic action and generates line style
Polyurethane acrylate prepolymer is made by oneself, wherein both features containing polyurethane in self-control polyurethane acrylate prepolymer molecule
Group-NHCOOR, and the double bond with polymerization activity containing esters of acrylic acid, occur radical polymerization under the action of high temperature
It closes, makes crosslinking curing between polyurethane acrylates macromolecular chain, so that its adhesive strength is improved, in addition make polyurethane by oneself
In acrylic ester prepolymer molecule contain active isocyanate groups, when exposed to air, can with it is micro in air
Moisture reacts, and in bonding, it can occur with hydroxyl isoreactivity group existing for the water of substrate surface absorption and surface
Chemical reaction generates urea bond structure, and the adhesive strength and water proofing property for being conducive to interfacial agents are improved, and recycles dodecyl sulphur
Sour sodium is modified the nano silicon dioxide of water resistance, makes nano silicon dioxide uniform adsorption in substrate surface, in high-speed stirring
During mixing, lauryl sodium sulfate has compatibilization to nano silicon dioxide, and the interface of nano silicon dioxide and base material is made to tie
Resultant force is improved, and also improves dispersibility and the physical crosslinking effect of nano silicon dioxide, while nano-silica surface
There are a large amount of unsaturated bonds and high activity hydroxyl, bonding action can occur with the polar group in base material, increase polymer
Crosslink density hinders moisture penetrating in the substrate, improves interfacial agents again to form fine and close three-dimensional net structure
Water proofing property;
(2)The present invention is by white carbon and the tetradecane hybrid reaction under vacuum so that and the tetradecane is adsorbed on white carbon surface,
Shaping phase-change material is obtained, and shaping phase-change material is mixed in concrete, when pavement temperature is reduced close to the phase of phase-change material
When height, Liquid-solid conversion will occur for liquid phase change material, this process can discharge a large amount of heat, using this heat prevent or
Concrete liquid is delayed to freeze, while base material or inside concrete hole are partially filled with by powdered shaping phase-change material, from
And the compactness of base material or concrete is improved, porosity is reduced, outside moisture hardly enters base material or inside concrete, separately
The incorporation of outer shaping phase-change material increases the thickness of base material or concrete, reduces the penetration capacity of moisture, to improve base
The freeze-thaw split intensity of material or concrete, the freeze-thaw resistance and water proofing property for being conducive to interfacial agents are improved, and continue to add coconut
Oil and ammonium carbonate, aliphatic acid in coconut oil is molecule separate out by ion transit, and is adsorbed at the active site of base material, is prevented
Only freeze thawing further occurs, and to extend the service life of interfacial agents, ammonium carbonate is in addition added into base material, had been stirred to react
Cheng Zhong is easy degradation and generates carboxylic acid, the An Deng functional groups that can more reduce freezing point, and further functioning as prevents from freezing, melts ice
The effect of snow, is with a wide range of applications.
Specific implementation mode
50~60mL polycaprolactone glycols are weighed to be added in the four-hole boiling flask equipped with blender, thermometer and condenser pipe,
12~16min is stirred at being 95~100 DEG C in temperature, after stirring, and is subtracted under conditions of pressure is 0.06~0.08MPa
21~25min of press-dehydrating obtains stirring thing, continues to be 5 in mass ratio:2:2:1 by stirring thing, hydroxy-ethyl acrylate, to benzene two
The hydrogen peroxide mixing that phenol and mass fraction are 26% is placed in beaker, and 1~2h is stirred to react at being 53~64 DEG C in temperature, cooling
Discharging obtains self-control polyurethane acrylate prepolymer;It is 2 by volume:4:1 by deionized water, ethyl orthosilicate and anhydrous
Ethyl alcohol mixing is placed in beaker, is stirred 12~16min at being 50~52 DEG C in temperature, is obtained stirring liquid, then be added dropwise into beaker
The hydrochloric acid that the mass fraction of agitated liquid product 0.5% is 24% continues to keep the temperature 21~27min of hybrid reaction, reaction solution is obtained, by matter
Amount is than being 4:1 is put into reaction solution and lauryl sodium sulfate mixing in ultrasonic wave separating apparatus, in the item that frequency is 24~32kHz
35~45min of ultrasonic disperse under part, after ultrasonic disperse, still aging 1~2 day, discharging was obtained from preparing silicon collosol;By etc.
White carbon and the tetradecane are mixed and are placed in vacuum pump by mass ratio, under conditions of pressure is 0.06~0.08Mpa reaction 16~
20min so that the tetradecane is adsorbed on white carbon surface, and grinding discharging obtains shaping phase-change material powder;It counts in parts by weight,
Weigh that 35~45 parts of self-control polyurethane acrylate prepolymers, 12~16 parts from preparing silicon collosol, 6~8 parts of fixed phase change materials respectively
Material and 24~32 parts of deionized water mixing are placed in blender, stir 35~45min at being 45~55 DEG C in temperature, then add 2
~4 parts of absolute ethyl alcohols, 1~3 part of silicone emulsion, 3~5 portions of coconut oil and 2~4 parts of ammonium carbonates, temperature be 75~85 DEG C at after
Continuous that 1~2h is mixed, cooling discharging is to get freeze proof melt type watertight interface agent.
Example 1
It weighs 50mL polycaprolactone glycols to be added in the four-hole boiling flask equipped with blender, thermometer and condenser pipe, is in temperature
12min is stirred at 95 DEG C, after stirring, and decompression dehydration 21min under conditions of pressure is 0.06MPa, stirring thing is obtained,
Continue to be 5 in mass ratio:2:2:1 mixes the hydrogen peroxide that stirring thing, hydroxy-ethyl acrylate, hydroquinone and mass fraction are 26%
Conjunction is placed in beaker, and 1h is stirred to react at being 53 DEG C in temperature, and cooling discharging obtains self-control polyurethane acrylate prepolymer;
It is 2 by volume:4:1 is placed in the mixing of deionized water, ethyl orthosilicate and absolute ethyl alcohol in beaker, is stirred at being 50 DEG C in temperature
12min is mixed, stirring liquid is obtained, then the hydrochloric acid that the mass fraction of agitated liquid product 0.5% is 24% is added dropwise into beaker, continues to keep the temperature
Hybrid reaction 21min obtains reaction solution, is in mass ratio 4:Reaction solution and lauryl sodium sulfate mixing are put into ultrasonic wave by 1
In separating apparatus, ultrasonic disperse 35min under conditions of frequency is 24kHz, after ultrasonic disperse, still aging 1 day, discharging,
It obtains from preparing silicon collosol;White carbon and the tetradecane are mixed by equal mass ratioes and are placed in vacuum pump, in the item that pressure is 0.06Mpa
16min is reacted under part so that the tetradecane is adsorbed on white carbon surface, and grinding discharging obtains shaping phase-change material powder;By weight
Number meter, weigh respectively 35 parts self-control polyurethane acrylate prepolymers, 12 parts from preparing silicon collosol, 6 parts of shaping phase-change materials and
24 parts of deionized water mixing are placed in blender, stir 35min at being 45 DEG C in temperature, then add 2 parts of absolute ethyl alcohols, 1 part of breast
SiClx oil, 3 portions of coconut oil and 2 parts of ammonium carbonates at being 75 DEG C in temperature continue that 1h is mixed, and cooling discharging is to get freeze thawing resistance
Type watertight interface agent.
Example 2
It weighs 55mL polycaprolactone glycols to be added in the four-hole boiling flask equipped with blender, thermometer and condenser pipe, is in temperature
14min is stirred at 98 DEG C, after stirring, and decompression dehydration 23min under conditions of pressure is 0.07MPa, stirring thing is obtained,
Continue to be 5 in mass ratio:2:2:1 mixes the hydrogen peroxide that stirring thing, hydroxy-ethyl acrylate, hydroquinone and mass fraction are 26%
Conjunction is placed in beaker, and 1.5h is stirred to react at being 58 DEG C in temperature, and it is poly- to obtain self-control polyurethane acrylate prepolymer for cooling discharging
Object;It is 2 by volume:4:1 is placed in the mixing of deionized water, ethyl orthosilicate and absolute ethyl alcohol in beaker, is 51 DEG C in temperature
Lower stirring 14min obtains stirring liquid, then the hydrochloric acid that the mass fraction of agitated liquid product 0.5% is 24% is added dropwise into beaker, continues
Hybrid reaction 24min is kept the temperature, reaction solution is obtained, is in mass ratio 4:1 reaction solution and lauryl sodium sulfate are mixed be put into it is super
In sound wave separating apparatus, ultrasonic disperse 40min under conditions of frequency is 28kHz, after ultrasonic disperse, still aging 1.5 days,
Discharging, obtains from preparing silicon collosol;White carbon and the tetradecane are mixed by equal mass ratioes and are placed in vacuum pump, is in pressure
18min is reacted under conditions of 0.07Mpa so that the tetradecane is adsorbed on white carbon surface, and grinding discharging obtains shaping phase-change material
Powder;Count in parts by weight, weigh respectively 40 parts self-control polyurethane acrylate prepolymers, 14 parts from preparing silicon collosol, 7 parts setting
Phase-change material and the mixing of 28 parts of deionized waters are placed in blender, and 40min is stirred at being 50 DEG C in temperature, then add 3 parts it is anhydrous
Ethyl alcohol, 2 parts of silicone emulsions, 4 portions of coconut oil and 3 parts of ammonium carbonates continue that 1.5h is mixed at being 80 DEG C in temperature, and cooling goes out
Material is to get freeze proof melt type watertight interface agent.
Example 3
It weighs 60mL polycaprolactone glycols to be added in the four-hole boiling flask equipped with blender, thermometer and condenser pipe, is in temperature
16min is stirred at 100 DEG C, after stirring, and decompression dehydration 25min under conditions of pressure is 0.08MPa, it is stirred
Object continues to be 5 in mass ratio:2:2:1 by stirring thing, hydroxy-ethyl acrylate, hydroquinone and mass fraction be 26% hydrogen peroxide
Mixing is placed in beaker, and 2h is stirred to react at being 64 DEG C in temperature, and it is poly- to obtain self-control polyurethane acrylate prepolymer for cooling discharging
Object;It is 2 by volume:4:1 is placed in the mixing of deionized water, ethyl orthosilicate and absolute ethyl alcohol in beaker, is 52 DEG C in temperature
Lower stirring 16min obtains stirring liquid, then the hydrochloric acid that the mass fraction of agitated liquid product 0.5% is 24% is added dropwise into beaker, continues
Hybrid reaction 27min is kept the temperature, reaction solution is obtained, is in mass ratio 4:1 reaction solution and lauryl sodium sulfate are mixed be put into it is super
In sound wave separating apparatus, ultrasonic disperse 45min under conditions of frequency is 32kHz after ultrasonic disperse, still aging 2 days, goes out
Material, obtains from preparing silicon collosol;White carbon and the tetradecane are mixed by equal mass ratioes and are placed in vacuum pump, is 0.08Mpa in pressure
Under conditions of react 20min so that the tetradecane is adsorbed on white carbon surface, and grinding discharging obtains shaping phase-change material powder;It presses
Parts by weight meter, weighs that 45 parts of self-control polyurethane acrylate prepolymers, 16 parts from preparing silicon collosol, 8 parts of fixed phase change materials respectively
Material and 32 parts of deionized water mixing are placed in blender, stir 45min at being 55 DEG C in temperature, then add 4 parts of absolute ethyl alcohols, 3
Part silicone emulsion, 5 portions of coconut oil and 4 parts of ammonium carbonates continue that 2h is mixed at being 85 DEG C in temperature, and cooling discharging is to get anti-
Frost thawing type watertight interface agent.
Comparative example
As a comparison case with the interfacial agents of company of Jinan City production
Interfacial agents in freeze proof melt type watertight interface agent produced by the present invention and comparative example are detected, testing result such as table 1
It is shown:
1, adhesion strength is tested
It is tested by 6.13 standards in JG/T157-2004.
2, shear viscosity is tested
It is tested by 6.3.4 standards in JG/T574.
3, impermeability is tested
By in GB/T1677 11 method test.
1 performance measurement result of table
From the data in table 1, it can be seen that freeze proof melt type watertight interface agent produced by the present invention, with adhesive property is good, water resistance is strong, resistance to jelly
Melting property is good, will not freeze under -20 DEG C of environment, be placed on it is outdoor be exposed to the sun by 7 days, and drenched with rain, the natural erosions such as wind, appearance without
Significant change has good market prospects.
Claims (5)
1. a kind of preparation method of freeze proof melt type watertight interface agent, it is characterised in that specifically preparation process is:
(1)It weighs 50~60mL polycaprolactone glycols and is added in the four-hole boiling flask equipped with blender, thermometer and condenser pipe and stir
It mixes, after stirring, and decompression dehydration, stirring thing is obtained, is continued stirring thing, hydroxy-ethyl acrylate, hydroquinone and dioxygen
Water mixing, which is placed in beaker, to be stirred to react, and cooling discharging obtains self-control polyurethane acrylate prepolymer;
(2)Deionized water, ethyl orthosilicate and absolute ethyl alcohol are mixed and is placed in beaker and stirs, obtains stirring liquid, then to beaker
The middle hydrochloric acid that agitated liquid product 0.5% is added dropwise, continues to keep the temperature hybrid reaction, reaction solution is obtained, by reaction solution and dodecyl sulphate
Sodium, which mixes, is put into ultrasonic disperse in ultrasonic wave separating apparatus, still aging after ultrasonic disperse, and discharging is obtained from preparing silicon collosol;
(3)White carbon and the tetradecane are mixed to be placed in vacuum pump by equal mass ratioes and reacted so that the tetradecane is adsorbed on white carbon
Surface, grinding discharging, obtains shaping phase-change material powder;
(4)It counts in parts by weight, weighs 35~45 parts of self-control polyurethane acrylate prepolymers, 12~16 parts of self-control silicon respectively
Colloidal sol, 6~8 parts of shaping phase-change materials and 24~32 parts of deionized water mixing are placed in blender and stir, then add 2~4 parts of nothings
Water-ethanol, 1~3 part of silicone emulsion, 3~5 portions of coconut oil and 2~4 parts of ammonium carbonates, continue to be mixed, and cooling discharging is to get anti-
Frost thawing type watertight interface agent.
2. a kind of preparation method of freeze proof melt type watertight interface agent according to claim 1, it is characterised in that:Step(1)
The whipping temp is 95~100 DEG C, and mixing time is 12~16min, and decompression dehydration pressure is 0.06~0.08Mpa, is subtracted
The press-dehydrating time is 21~25min, the matter for the hydrogen peroxide that stirring thing, hydroxy-ethyl acrylate, hydroquinone and mass fraction are 26%
Amount is than being 5:2:2:1, it is 53~64 DEG C to be stirred to react temperature, and it is 1~2h to be stirred to react the time.
3. a kind of preparation method of freeze proof melt type watertight interface agent according to claim 1, it is characterised in that:Step(2)
The volume ratio of the deionized water, ethyl orthosilicate and absolute ethyl alcohol is 2:4:1, whipping temp is 50~52 DEG C, when stirring
Between be 12~16min, the mass fraction of hydrochloric acid is 24%, and the reaction was continued, and the time is 21~27min, reaction solution and dodecyl sulphur
The mass ratio of sour sodium is 4:1, ultrasonic disperse frequency is 24~32kHz, and the ultrasonic disperse time is 35~45min, when still aging
Between be 1~2 day.
4. a kind of preparation method of freeze proof melt type watertight interface agent according to claim 1, it is characterised in that:Step(3)
The reaction pressure is 0.06~0.08Mpa, and the reaction time is 16~20min.
5. a kind of preparation method of freeze proof melt type watertight interface agent according to claim 1, it is characterised in that:Step(4)
The whipping temp is 45~55 DEG C, and mixing time is 35~45min, and it is 75~85 DEG C to continue whipping temp, continues to stir
Time is 1~2h.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109610705A (en) * | 2018-12-04 | 2019-04-12 | 江苏兴厦建设工程集团有限公司 | It is a kind of control toilet ship-and-galley tile hollowing, cracking, leakage construction method |
FR3141158A1 (en) * | 2022-10-25 | 2024-04-26 | Arkema France | Hydrogen peroxide production process |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102559038A (en) * | 2012-02-16 | 2012-07-11 | 长沙市原鹏化工科技有限公司 | Organosilicon-modified polyurethane-acrylic ester photocurable coating and preparation method thereof |
-
2018
- 2018-02-10 CN CN201810137605.3A patent/CN108395833A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102559038A (en) * | 2012-02-16 | 2012-07-11 | 长沙市原鹏化工科技有限公司 | Organosilicon-modified polyurethane-acrylic ester photocurable coating and preparation method thereof |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109610705A (en) * | 2018-12-04 | 2019-04-12 | 江苏兴厦建设工程集团有限公司 | It is a kind of control toilet ship-and-galley tile hollowing, cracking, leakage construction method |
FR3141158A1 (en) * | 2022-10-25 | 2024-04-26 | Arkema France | Hydrogen peroxide production process |
WO2024089347A1 (en) * | 2022-10-25 | 2024-05-02 | Arkema France | Method for producing hydrogen peroxide |
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