CN108299930A - A kind of preparation method of nano-silicon delustering agent - Google Patents
A kind of preparation method of nano-silicon delustering agent Download PDFInfo
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
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- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
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- 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
- C08K3/02—Elements
- C08K3/04—Carbon
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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- C—CHEMISTRY; METALLURGY
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Abstract
The present invention relates to a kind of preparation methods of nano-silicon delustering agent, belong to delustering agent preparing technical field.Ash content silica is not contained only in rice hull ash of the present invention, the also wood fibre of charred rice husk, in micro- carbonization process, magnesium powder can soon combustion oxidation at magnesia, it is adsorbed in the micropore of carbonized wooden fiber, for coated with silica in carbonized wooden fibrous inside, the magnesia crystal grain size on extinction material surface is smaller, more dense uniform is arranged, thus feel is preferable；In extinction material made of delustering agent of the present invention, after light is by magnesia crystal, refract to carbon-coating, reach the nano grain surface of silica, energy is largely absorbed by carbon-coating in the form of molecular motion, finally since the diffusing reflection of maximum probability occurs for the small particle of silica, to reach splendid extinction effect.
Description
Technical field
The present invention relates to a kind of preparation methods of nano-silicon delustering agent, belong to delustering agent preparing technical field.
Background technology
Delustering agent is one kind of white carbon, is produced by the method for chemical reactive synthesis, is a kind of unformed micron order
Superfine silicon dioxide particle.Applied to oiliness, the surface of aqueous and powder-type coating, ink system and plastic cement, aluminium the first day of the lunar month product
Deng playing photoextinction.
Existing extinction method is mainly physics delustring and chemical quenching two ways.Physics delustring is added in coating
Delustering agent makes its surface irregularity in film forming procedure, increases the scattering to light and reduces and reflect, to generate delustring effect
Fruit.The main extinction material of physics delustring is made of metallic soap, functional fines and wax three categories, wherein belongs to functional
Synthetic silica in fines is presently most popular also the most general extinction material.Physics delustring has apparent delustring
Effect, but that there is also feels is poor, the shortcomings of conjunction loosely with leather block.
Chemical quenching be positioned against the light-absorbing structure of energy that some for example polypropylene grafted substance classes are introduced in coating or
Group, to obtain low gloss.Currently on the market leather surface using it is more be solvent type polyurethane resin gloss oil, but these light
There is limitation in use due to environmental problem in oil.Aqueous polyurethane extinction material is used for leather top finishing physical property
It is good, comfortable feel, and with energy-saving and environmental protection, simple operation and other advantages, paid attention to by leather industry.
Especially the environmental consciousness of people constantly enhances in recent years, and this facilitate the exploitations of water-base polyurethane material, but at present
The aqueous polyurethane extinction material used in the market, extinction performance are weaker than physics delustering agent mostly, to reach stronger delustring effect
Fruit is typically necessary and additionally adds the physics delustering agents such as silica to realize, and the addition of physics delustering agent can be to aqueous poly-
The feel and physical and chemical performance of urethane extinction material itself have adverse effect on.
Therefore, a kind of extinction effect and the extinction material of feel of capable of taking into account of invention has positive meaning.
Invention content
Present invention mainly solves the technical issues of, cannot be taken into account for the feel of delustering agent extinction effect and extinction material
Defect provides a kind of preparation method of nano-silicon delustering agent.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of nanometer silica gel delustering agent, it is characterised in that specifically preparation process is：
（1）600~800g rice husks are weighed, rice husk is lighted and obtains rice hull ash, rice hull ash is added in glass guide channel, are added into glass guide channel
Enter 500~600mL sodium hydroxide solutions and impregnate rice hull ash, after immersion, then the sulfuric acid of 600~800mL of addition is molten into glass guide channel
Liquid, heat temperature raising start blender and stir, and after insulation reaction, filtering removal filter residue obtains gel；
（2）Gel is washed with deionized, then the gel after washing is put into baking oven, heat temperature raising, is done after dry
Xerogel is placed in high-pressure pulse nano-scale crusher by gel, after crushing, obtains nanogel powder；
（3）Nanogel powder is mixed with magnesium powder, mixture is obtained, mixture is put into retort, heat temperature raising is kept the temperature micro-
Charing, obtains micro- charing powder；
（4）It counts in parts by weight, 10~15 parts of polytetrahydrofuran diols, 20~30 parts of micro- carbonization powers is added to four round flask
5~10 parts of works are added dropwise with constant pressure funnel in end, 30~40 parts of dihydromethyl propionic acids, heat temperature raising, vacuum drying, cooling
Industry grade bismuthic acid starts blender stirring and adds 20~30 parts of isophorone diisocyanate after stirring 10~15min, heats
Heating after reaction, is cooled to room temperature discharging, obtains a kind of nanometer silica gel delustering agent.
Step（1）The mass fraction of the sodium hydroxide solution is 30%, and soaking time is 10~15min, sulfuric acid solution
Mass fraction be 20%, temperature is 90~100 DEG C after heat temperature raising, and speed of agitator is 70~80r/min, insulation reaction time
For 20~30min.
Step（2）The washing times are 3~5 times, and temperature is 100~110 DEG C after heat temperature raising, drying time 45
~55min, grinding time are 10~15min.
Step（3）The nanogel powder and magnesium powder mixing quality ratio are 3 ﹕ 1, and temperature is 300~350 after heat temperature raising
DEG C, it is 30~40min to keep the temperature micro- carbonization time.
Step（4）After the first time heat temperature raising temperature be 100~110 DEG C, the vacuum drying time be 1.0~
1.5h, after cooling temperature be 40~50 DEG C, constant pressure funnel drop rate be 1~3mL/min, agitator speed be 150~
170r/min, temperature is 80~85 DEG C after second of heat temperature raising, and the reaction time is 2~3h.
Beneficial effects of the present invention：
（1）Ash content silica, the also wood fibre of charred rice husk are not contained only in rice hull ash of the present invention, in micro- carbonization process
In, magnesium powder combustion oxidation can be adsorbed at magnesia in the micropore of carbonized wooden fiber soon, and coated with silica is carbonizing
Inside wood fibre, the magnesia crystal grain size on extinction material surface is smaller, arranges more dense uniform, thus feel is preferable；
（2）In extinction material made of delustering agent of the present invention, after light is by magnesia crystal, carbon-coating is refracted to, reaches dioxy
The nano grain surface of SiClx, energy are largely absorbed by carbon-coating in the form of molecular motion, finally small due to silica
The diffusing reflection of maximum probability occurs for grain size, to reach splendid extinction effect.
Specific implementation mode：
600~800g rice husks are weighed, rice husk is lighted and obtains rice hull ash, rice hull ash is added in glass guide channel, is added into glass guide channel
The sodium hydroxide solution that 500~600mL mass fractions are 30% impregnates rice hull ash, after impregnating 10~15min, then into glass guide channel
The sulfuric acid solution that 600~800mL mass fractions are 20% is added, is heated to 90~100 DEG C, start blender with 70~
80r/min rotating speeds stir, and after 20~30min of insulation reaction, filtering removal filter residue obtains gel；Gel is washed with deionized
3~5 times, then the gel after washing is put into baking oven, 100~110 DEG C are heated to, dry 45~55min obtains dry solidifying
Xerogel is placed in high-pressure pulse nano-scale crusher by glue, after crushing 10~15min, obtains nanogel powder；By nanogel
Powder is that 3 ﹕ 1 are mixed in mass ratio with magnesium powder, obtains mixture, mixture is put into retort, be heated to 300~350
DEG C, 30~40min of micro- charing is kept the temperature, micro- charing powder is obtained；It counts in parts by weight, 10~15 parts is added to four round flask
Polytetrahydrofuran diol, 20~30 parts of micro- charing powder, 30~40 parts of dihydromethyl propionic acids, are heated to 100~110 DEG C,
1.0~1.5h of vacuum drying is cooled to 40~50 DEG C, and 5~10 parts of industry are added dropwise with 1~3mL/min with constant pressure funnel
Grade bismuthic acid is started blender and is stirred with 150~170r/min rotating speeds, after stirring 10~15min, adds 20~30 parts of different Fo Er
Ketone diisocyanate, is heated to 80~85 DEG C, after reacting 2~3h, is cooled to room temperature discharging, obtains a kind of nanometer silica gel and disappears
Photo etching.
Example 1
600g rice husks are weighed, rice husk is lighted and obtains rice hull ash, rice hull ash is added in glass guide channel, 500mL is added into glass guide channel
The sodium hydroxide solution that mass fraction is 30% impregnates rice hull ash, after impregnating 10min, then 600mL mass point is added into glass guide channel
Number is 20% sulfuric acid solution, is heated to 90 DEG C, starts blender and is stirred with 70r/min rotating speeds, after insulation reaction 20min,
Filtering removal filter residue obtains gel；Gel is washed with deionized 3 times, then the gel after washing is put into baking oven, is heated
100 DEG C are warming up to, dry 45min obtains xerogel, and xerogel is placed in high-pressure pulse nano-scale crusher, after crushing 10min,
Obtain nanogel powder；Nanogel powder is mixed for 3 ﹕ 1 in mass ratio with magnesium powder, mixture is obtained, mixture is put into charcoal
Change in stove, is heated to 300 DEG C, keeps the temperature micro- charing 30min, obtain micro- charing powder；It counts in parts by weight, to four mouthfuls of round bottoms
10 parts of polytetrahydrofuran diols, 20 parts of micro- charing powder, 30 parts of dihydromethyl propionic acids are added in flask, are heated to 100 DEG C, take out
Be dried in vacuo 1.0h, be cooled to 40 DEG C, with constant pressure funnel with 1mL/min be added dropwise 5 parts of technical grade bismuthic acids, start blender with
150r/min rotating speeds stir, and after stirring 10min, add 20 parts of isophorone diisocyanate, are heated to 80 DEG C, reaction
After 2h, it is cooled to room temperature discharging, obtains a kind of nanometer silica gel delustering agent.
Example 2
700g rice husks are weighed, rice husk is lighted and obtains rice hull ash, rice hull ash is added in glass guide channel, 550mL is added into glass guide channel
The sodium hydroxide solution that mass fraction is 30% impregnates rice hull ash, after impregnating 13min, then 700mL mass point is added into glass guide channel
Number is 20% sulfuric acid solution, is heated to 95 DEG C, starts blender and is stirred with 75r/min rotating speeds, after insulation reaction 25min,
Filtering removal filter residue obtains gel；Gel is washed with deionized 4 times, then the gel after washing is put into baking oven, is heated
105 DEG C are warming up to, dry 50min obtains xerogel, and xerogel is placed in high-pressure pulse nano-scale crusher, after crushing 13min,
Obtain nanogel powder；Nanogel powder is mixed for 3 ﹕ 1 in mass ratio with magnesium powder, mixture is obtained, mixture is put into charcoal
Change in stove, is heated to 330 DEG C, keeps the temperature micro- charing 35min, obtain micro- charing powder；It counts in parts by weight, to four mouthfuls of round bottoms
13 parts of polytetrahydrofuran diols, 25 parts of micro- charing powder, 35 parts of dihydromethyl propionic acids are added in flask, are heated to 105 DEG C, take out
Be dried in vacuo 1.3h, be cooled to 45 DEG C, with constant pressure funnel with 2mL/min be added dropwise 8 parts of technical grade bismuthic acids, start blender with
160r/min rotating speeds stir, and after stirring 13min, add 25 parts of isophorone diisocyanate, are heated to 83 DEG C, reaction
After 2h, it is cooled to room temperature discharging, obtains a kind of nanometer silica gel delustering agent.
Example 3
800g rice husks are weighed, rice husk is lighted and obtains rice hull ash, rice hull ash is added in glass guide channel, 600mL is added into glass guide channel
The sodium hydroxide solution that mass fraction is 30% impregnates rice hull ash, after impregnating 15min, then 800mL mass point is added into glass guide channel
Number is 20% sulfuric acid solution, is heated to 100 DEG C, starts blender and is stirred with 80r/min rotating speeds, insulation reaction 30min
Afterwards, filtering removal filter residue obtains gel；Gel is washed with deionized 5 times, then the gel after washing is put into baking oven, is added
Heat is warming up to 110 DEG C, and dry 55min obtains xerogel, and xerogel is placed in high-pressure pulse nano-scale crusher, crushes 15min
Afterwards, nanogel powder is obtained；Nanogel powder is mixed for 3 ﹕ 1 in mass ratio with magnesium powder, mixture is obtained, mixture is put into
In retort, 350 DEG C are heated to, keeps the temperature micro- charing 40min, obtains micro- charing powder；It counts in parts by weight, to four mouthfuls of circles
15 parts of polytetrahydrofuran diols, 30 parts of micro- charing powder, 40 parts of dihydromethyl propionic acids are added in bottom flask, are heated to 110 DEG C,
Vacuum drying 1.5h is cooled to 50 DEG C, and 10 parts of technical grade bismuthic acids are added dropwise with 3mL/min with constant pressure funnel, start stirring
Device is stirred with 170r/min rotating speeds, after stirring 15min, is added 30 parts of isophorone diisocyanate, is heated to 85 DEG C,
After reacting 3h, it is cooled to room temperature discharging, obtains a kind of nanometer silica gel delustering agent.
Reference examples
With the delustering agent example as a contrast of Nanjing company production
It is sprayed on substrate after being mixed delustering agent and coating using the method for electrostatic spraying, is toasted at 180 DEG C respectively
The film that film thickness is 60~70 μm is made in 15min, solidification, and 60 ° of lower coating gloss, detection are detected with BYKAG-4450 type glossometers
The results are shown in Table 1：
Table 1
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Gloss（60°）（%） | 8.5 | 8.3 | 8.0 | 20.1 |
| Roughness（μm） | 400 | 405 | 410 | 950 |
By detection data in upper table it is found that delustering agent produced by the present invention has both extinction effect and good feel simultaneously, have
Splendid application prospect.
Claims (5)
1. a kind of preparation method of nanometer silica gel delustering agent, it is characterised in that specifically preparation process is：
（1）600~800g rice husks are weighed, rice husk is lighted and obtains rice hull ash, rice hull ash is added in glass guide channel, are added into glass guide channel
Enter 500~600mL sodium hydroxide solutions and impregnate rice hull ash, after immersion, then the sulfuric acid of 600~800mL of addition is molten into glass guide channel
Liquid, heat temperature raising start blender and stir, and after insulation reaction, filtering removal filter residue obtains gel；
（2）Gel is washed with deionized, then the gel after washing is put into baking oven, heat temperature raising, is done after dry
Xerogel is placed in high-pressure pulse nano-scale crusher by gel, after crushing, obtains nanogel powder；
（3）Nanogel powder is mixed with magnesium powder, mixture is obtained, mixture is put into retort, heat temperature raising is kept the temperature micro-
Charing, obtains micro- charing powder；
（4）It counts in parts by weight, 10~15 parts of polytetrahydrofuran diols, 20~30 parts of micro- carbonization powers is added to four round flask
5~10 parts of works are added dropwise with constant pressure funnel in end, 30~40 parts of dihydromethyl propionic acids, heat temperature raising, vacuum drying, cooling
Industry grade bismuthic acid starts blender stirring and adds 20~30 parts of isophorone diisocyanate after stirring 10~15min, heats
Heating after reaction, is cooled to room temperature discharging, obtains a kind of nanometer silica gel delustering agent.
2. a kind of preparation method of nanometer silica gel delustering agent according to claim 1, it is characterised in that：Step（1）It is described
The mass fraction of sodium hydroxide solution be 30%, soaking time is 10~15min, and the mass fraction of sulfuric acid solution is 20%, is added
Temperature is 90~100 DEG C after heat heating, and speed of agitator is 70~80r/min, and the insulation reaction time is 20~30min.
3. a kind of preparation method of nanometer silica gel delustering agent according to claim 1, it is characterised in that：Step（2）It is described
Washing times be 3~5 times, temperature is 100~110 DEG C after heat temperature raising, and drying time is 45~55min, and grinding time is
10~15min.
4. a kind of preparation method of nanometer silica gel delustering agent according to claim 1, it is characterised in that：Step（3）It is described
Nanogel powder and magnesium powder mixing quality ratio be 3 ﹕ 1, temperature is 300~350 DEG C after heat temperature raising, and keeping the temperature micro- carbonization time is
30~40min.
5. a kind of preparation method of nanometer silica gel delustering agent according to claim 1, it is characterised in that：Step（4）It is described
First time heat temperature raising after temperature be 100~110 DEG C, the vacuum drying time be 1.0~1.5h, after cooling temperature be 40
~50 DEG C, constant pressure funnel drop rate is 1~3mL/min, and agitator speed is 150~170r/min, second of heating
Temperature is 80~85 DEG C after heating, and the reaction time is 2~3h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109135492A (en) * | 2018-08-02 | 2019-01-04 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of anti-dazzle waterproof High tailored coating |
| CN110016278A (en) * | 2019-03-06 | 2019-07-16 | 常州市三伊化工有限公司 | A kind of preparation method of the anti-scratch black finish of dumb light |
| CN110305519A (en) * | 2019-06-12 | 2019-10-08 | 王银梅 | A kind of preparation method of high grade of transparency flatting silica |
| CN113716624A (en) * | 2021-08-31 | 2021-11-30 | 蜂巢能源科技有限公司 | Composite material, preparation method thereof and lithium ion battery anode material |
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| CN1762802A (en) * | 2005-09-09 | 2006-04-26 | 四川省宜宾五粮液集团有限公司 | Method for industrial production of white carbon black using rice husk |
| CN103319682A (en) * | 2013-07-11 | 2013-09-25 | 清远市美乐仕油墨有限公司 | Low-luster aqueous polyurethane dispersion for leather, and preparation method and application thereof |
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2017
- 2017-09-16 CN CN201710835828.2A patent/CN108299930A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1762802A (en) * | 2005-09-09 | 2006-04-26 | 四川省宜宾五粮液集团有限公司 | Method for industrial production of white carbon black using rice husk |
| CN103319682A (en) * | 2013-07-11 | 2013-09-25 | 清远市美乐仕油墨有限公司 | Low-luster aqueous polyurethane dispersion for leather, and preparation method and application thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109135492A (en) * | 2018-08-02 | 2019-01-04 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of anti-dazzle waterproof High tailored coating |
| CN110016278A (en) * | 2019-03-06 | 2019-07-16 | 常州市三伊化工有限公司 | A kind of preparation method of the anti-scratch black finish of dumb light |
| CN110305519A (en) * | 2019-06-12 | 2019-10-08 | 王银梅 | A kind of preparation method of high grade of transparency flatting silica |
| CN113716624A (en) * | 2021-08-31 | 2021-11-30 | 蜂巢能源科技有限公司 | Composite material, preparation method thereof and lithium ion battery anode material |
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Application publication date: 20180720 |