CN107551963A - A kind of preparation method of industry silicasol - Google Patents
A kind of preparation method of industry silicasol Download PDFInfo
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- CN107551963A CN107551963A CN201710933591.1A CN201710933591A CN107551963A CN 107551963 A CN107551963 A CN 107551963A CN 201710933591 A CN201710933591 A CN 201710933591A CN 107551963 A CN107551963 A CN 107551963A
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Abstract
The invention discloses a kind of preparation method of industry silicasol, belong to Ludox preparing technical field.The present invention mixes pigskin with water, freezes, and crushes, and sieves, and filters, and dries, obtains filter residue；After filter residue is mixed with sulfuric acid, heating stirring reaction, reaction product is obtained；By animal shell ball mill grinding, sieving, crust particle is obtained；Crust particle is mixed with hydrochloric acid heating stirring, filters, produces acid treatment filter residue；By acid treatment filter residue and sodium hydroxide solution heating stirring, pH is adjusted, is filtered, washing, produces filter cake；Filter cake is mixed with ethanol, heating stirring backflow, filtering, is concentrated under reduced pressure, produces crust extract solution；By silica flour, sodium hydroxide solution, water, reaction product, crust extract solution, silane coupler mixing, stirring reaction, it is concentrated under reduced pressure, produces industry silicasol.Industry silicasol provided by the invention has excellent performance, and it is big to be effectively prevented from the membrane rigidity of Ludox formation, is easily cracked, the problem of gloss difference.
Description
Technical field
The invention discloses a kind of preparation method of industry silicasol, belong to Ludox preparing technical field.
Background technology
Ludox category colloidal solution is odorless, nontoxic.Ludox is nano level silica dioxide granule in water or in solvent
Dispersion liquid.Due to the SiO in Ludox2Containing substantial amounts of water and hydroxyl, therefore Ludox can also be expressed as mSiO2.nH2O。
Preparing Ludox has different approach.The most frequently used method has ion-exchange, the one-step hydrolysis method of silica flour one, silane hydrolyzate method etc..
Ludox can be used as various fire bonds, have the characteristics that cohesive force is strong, high temperature resistant；For coating work
Industry, coating can be made firm, and can dirt-resisting dustproof, ageing-resistant, fire prevention etc.；For shell hot investment casting, it can make that shell mould intensity is big, casting
Make it is highly polished, it is better than waterglass molding quality with its moulding, instead of silester moulding can reduce cost and improve operation bar
Part；Ludox has higher specific surface area, available for catalyst manufacture and catalyst carrier；For paper industry, glass can be used as
Glass paper antitack agent, photography paper pretreating reagent, bag of cement antilubricant etc.；As textile industry sizing agent, it and finish and use
Wool, the spinnability of the rabbit hair are managed, reduces broken end, prevents flyings, improves yield rate, increases economic benefit；As silicon steel sheet processing
Agent, kinescope dispersant, floor wax antiskid etc..
It is the inorganic coating of base-material with wide the advantages that low cost, low-carbon, environmental protection, high rigidity and high temperature resistant using Ludox
General research and application；But the shortcomings of film that Ludox is formed is present, and rigidity is big, be easily cracked, gloss difference, limits its application.
The defects of in order to make up Ludox, it can be modified with organic matter.It is well known that silicones is former as main chain, Si using Si-O-Si
The inorganic polymer of cross-linking type half of organic group is connected on son, integrates the characteristic of organic matter and inorganic matter, has excellent
Heat-resisting quantity, resistance to ag(e)ing and pliability etc., and it is similar to the structure of Ludox；So modification available for Ludox.Cause
This, is further studied Ludox, improves the pliability of Ludox, particularly significant.
The content of the invention
The present invention solves the technical problem of：For traditional Ludox rigidity it is big, be easily cracked the problem of, there is provided one
The preparation method of kind industry silicasol.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）By pigskin and water in mass ratio 1：20~1：After being mixed in 30 No. 1 beakers of addition, it is placed in refrigerator and freezes, must freeze
Block；
（2）Above-mentioned gained frozen block is placed in freezing crusher, crushed, sieving, produces crushed material；
（3）Above-mentioned gained crushed material is placed in No. 2 beakers, dissolved by heating, is filtered, dries, obtains filter residue；
（4）It is 1 in mass ratio by filter residue and sulfuric acid：5~1：After 10 mixing, it is placed in crucible, heating stirring reaction, production must be reacted
Thing；
（5）Animal shell is placed in ball mill, ball mill grinding, sieves, obtain crust particle；
（6）By above-mentioned gained crust particle and hydrochloric acid in mass ratio 1：50~1：100 add in No. 3 beakers, heating stirring mixing,
Filtering, produces acid treatment filter residue；
（7）By above-mentioned gained acid treatment filter residue and sodium hydroxide solution in mass ratio 1：50~1：100 add in three-necked flask, add
Thermal agitation mixes, then salt acid for adjusting pH is added dropwise, and filters, and washing, produces filter cake；
（8）By above-mentioned gained filter cake and ethanol in mass ratio 1：50~1：100 add in four-hole boiling flask, heating stirring backflow, mistake
Filter, is concentrated under reduced pressure, produces crust extract solution；
（9）Count in parts by weight, by 30~40 parts of silica flours, 30~40 parts of sodium hydroxide solutions, 100~120 parts of water, 10~20 parts
Reaction product, 10~20 parts of crust extract solutions, 10~20 parts of silane coupler mixing, stirring reaction, produce mixed slurry；
（10）By above-mentioned gained mixed slurry press filtration, it is concentrated under reduced pressure, produces industry silicasol.
Step（2）It is described to cross the sieve that grit number is 80~100 mesh.
Step（5）The animal shell is hodmadod, any one in snail shell or freshwater mussel shell.
Step（5）It is described to cross the sieve that grit number is 200~300 mesh.
Step（9）The silane coupler is silane resin acceptor kh-550, silane coupler KH-560 or silane coupler
Any one in KH-570.
The beneficial effects of the invention are as follows：
（1）Technical solution of the present invention is by adding the product of pigskin and concentrated sulfuric acid heating response, in use, first, silicon
Alkane coupling agent is the silane of the group simultaneously containing two kinds of different chemical property in molecule, wherein one containing siloxanes key
End be easy to Ludox surface action, therefore, the Ludox of inorganic phase can be connected to by pig by the bridging action of organosilicon
Skin and the product of concentrated sulfuric acid heating response, on the one hand, the toughness and intensity of system can be lifted, be effectively prevented from Ludox formation
Membrane rigidity is big, is easily cracked and the problem of gloss difference, and on the other hand, the product of pigskin and concentrated sulfuric acid heating response contains largely hydrophilic
Sex factor, there is good hydrophily and water-retaining property, can cross and promote the abundant aquation of system, form fine and close bright Ludox film；
（2）Technical solution of the present invention is by adding crust extract solution, and in use, crust extract solution can be used as and increase first
Thick dose, secondly, substantial amounts of amino is contained in animal shell extract solution, on the one hand, can be with containing a large amount of active groups in system
Chemical bonding is formed, strengthens the toughness and intensity of the three-dimensional network of sol system, is effectively prevented from the membrane rigidity of Ludox formation
Greatly, be easily cracked, the problem of gloss difference, on the other hand, due in Ludox countless micelles reunite caused by three-dimensional net structure deposit
In a large amount of pore structures, can there are part organic component or inorganic component in absorption system, therefore pigskin adds with the concentrated sulfuric acid after solidification
The product of thermal response can be filled out by crust extract solution to be disperseed to fill in these holes, the intensity of further system, is effectively prevented from silicon
The problem of membrane rigidity that colloidal sol is formed is big and is easily cracked.
Embodiment
By Pi Yushui in mass ratio 1：20~1：30 are added in No. 1 beaker, and 10~20min is stirred with glass bar, then by No. 1
Beaker is placed in 2~3h of freezing in refrigerator, obtains frozen block；Gained frozen block is placed in freezing crusher, crushed, crosses 80~100
Purpose is sieved, and produces crushed material；Gained crushed material is placed in No. 2 beakers, No. 2 beakers are moved into digital display tests the speed temperature constant magnetic stirring
It is 70~80 DEG C in temperature in device, under the conditions of rotating speed is 300~400r/min, heating stirring is melted to complete, obtains thawing solution,
Then thawing solution is filtered, obtains wet stock, then wet stock is placed in vacuum freezing drying oven and dries 40~50min, obtains filter residue；
Filter residue and mass fraction are pressed into quality 1 for 8~10% sulfuric acid：5~1：10 mixing after, be placed in crucible, in temperature be 120~
Under the conditions of 140 DEG C, and with glass bar 30~40min of stirring reaction, reaction product is produced；Animal shell is placed in ball mill,
Under the conditions of rotating speed is 500~600r/min, ball mill grinding, the sieve of 200~300 mesh is crossed, obtains crust particle；Gained crust is broken
Material and the hydrochloric acid in mass ratio 1 that mass fraction is 8~10%：50~1：100 are added in No. 3 beakers, then No. 3 beakers are moved into number
In the aobvious constant temperature blender with magnetic force that tests the speed, it is 70~80 DEG C in temperature, under the conditions of rotating speed is 300~400r/min, is stirred 20
After~30min, filtering, acid treatment filter residue is produced；Gained acid treatment filter residue is molten for 10~20% sodium hydroxide with mass fraction
Liquid in mass ratio 1：50~1：100 add in three-necked flasks, and three-necked flask then is moved into digital display tests the speed constant temperature blender with magnetic force
In, it is 70~80 DEG C in temperature, under the conditions of rotating speed is 300~400r/min, is stirred 30~40min, then use constant pressure addition
Mass fraction is added dropwise as 8~10% hydrochloric acid into three-necked flask using 2.5mL/min speed in funnel, and regulation pH is 7.1~7.3, is treated
Mass fraction be 8~10% hydrochloric acid solution be added dropwise after, filtering, obtain pretreated material, then by pretreated material spend from
Sub- water washing 3~5 times, produces filter cake；By gained filter cake and absolute ethyl alcohol in mass ratio 1：50~1：100 add four-hole boiling flask
In, then four-hole boiling flask is moved into digital display and tested the speed in constant temperature blender with magnetic force, it is 80~85 DEG C in temperature, rotating speed is 300~400r/
Under the conditions of min, heating stirring flows back after 40~50min, filtering, obtains filtrate, gained filtrate is placed in Rotary Evaporators, Yu Wen
Spend for 80~85 DEG C, pressure is 300~400kPa, and under the conditions of rotating speed is 60~80r/min, be concentrated under reduced pressure 10~20min, produces
Crust extract solution；Count in parts by weight, by 30~40 parts of silica flours, 30~40 parts of sodium hydroxide solutions, 100~120 parts of water, 10~
20 parts of reaction products, 10~20 parts of crust extract solutions, 10~20 parts of silane couplers are added in batch mixer, added in No. 4 beakers,
Under the conditions of rotating speed is 400~500r/min, 40~50min of reaction is stirred, produces mixed slurry；By gained mixed slurry
20~30min of press filtration in filter press is placed in, obtains press filtration slurry, then gained press filtration slurry is placed in Rotary Evaporators, Yu Wen
Spend for 100~110 DEG C, pressure is 300~400kPa, and under the conditions of rotating speed is 70~90r/min, be concentrated under reduced pressure 20~30min, subtracts
Pressure concentration, produces industry silicasol.The animal shell is hodmadod, any one in snail shell or freshwater mussel shell.The silicon
Alkane coupling agent is silane resin acceptor kh-550, any one in silane coupler KH-560 or Silane coupling reagent KH-570.
Example 1
By pigskin and water in mass ratio 1：30 add in No. 1 beaker, stir 20min with glass bar, then No. 1 beaker is placed in into refrigerator
Middle freezing 3h, obtains frozen block；Gained frozen block is placed in freezing crusher, crushed, the sieve of 100 mesh is crossed, produces crushed material；Will
Gained crushed material is placed in No. 2 beakers, and No. 2 beakers are moved into digital display tests the speed in constant temperature blender with magnetic force, is 80 DEG C in temperature, is turned
Under the conditions of speed is 400r/min, heating stirring is melted to complete, is obtained thawing solution, is then filtered thawing solution, obtains wet stock, then will
Wet stock, which is placed in vacuum freezing drying oven, dries 50min, obtains filter residue；Filter residue and mass fraction are pressed into quality for 10% sulfuric acid
1：10 mixing after, be placed in crucible, in temperature be 140 DEG C under the conditions of, and use glass bar stirring reaction 40min, produce reaction produce
Thing；Animal shell is placed in ball mill, under the conditions of rotating speed is 600r/min, ball mill grinding, the sieve of 300 mesh is crossed, obtains crust
Particle；By the hydrochloric acid in mass ratio 1 that gained crust particle and mass fraction are 10%：100 are added in No. 3 beakers, then No. 3 are burnt
Cup moves to digital display and tested the speed in constant temperature blender with magnetic force, is 80 DEG C in temperature, under the conditions of rotating speed is 400r/min, is stirred
After 30min, filtering, acid treatment filter residue is produced；Gained acid treatment filter residue and mass fraction are pressed into matter for 20% sodium hydroxide solution
Measure ratio 1：100 add in three-necked flasks, and three-necked flask then is moved into digital display tests the speed in constant temperature blender with magnetic force, in temperature be 80
DEG C, under the conditions of rotating speed is 400r/min, 40min is stirred, then burnt with 2.5mL/min speed to three mouthfuls with constant pressure funnel
The hydrochloric acid that mass fraction is 10% is added dropwise in bottle, regulation pH is 7.3, after the hydrochloric acid solution that mass fraction is 10% is added dropwise,
Filtering, obtains pretreated material, then pretreated material is washed with deionized 5 times, produces filter cake；By gained filter cake with it is anhydrous
Ethanol in mass ratio 1：100 are added in four-hole boiling flasks, then four-hole boiling flask is moved into digital display and tested the speed in constant temperature blender with magnetic force, Yu Wen
Spend for 85 DEG C, under the conditions of rotating speed is 400r/min, after heating stirring backflow 50min, filtering, obtains filtrate, gained filtrate is placed in
It it is 85 DEG C, pressure 400kPa in temperature, under the conditions of rotating speed is 80r/min, be concentrated under reduced pressure 20min, produces in Rotary Evaporators
Crust extract solution；Count in parts by weight, by 40 parts of silica flours, 40 parts of sodium hydroxide solutions, 120 parts of water, 20 parts of reaction products, 20 parts
Crust extract solution, 20 parts of silane couplers are added in batch mixer, added in No. 4 beakers, under the conditions of rotating speed is 500r/min, are stirred
Hybrid reaction 50min is mixed, produces mixed slurry；Gained mixed slurry is placed in press filtration 30min in filter press, obtains press filtration slurry,
Then gained press filtration slurry is placed in Rotary Evaporators, is 110 DEG C, pressure 400kPa in temperature, rotating speed is 90r/min bars
Under part, be concentrated under reduced pressure 30min, is concentrated under reduced pressure, and produces industry silicasol.The animal shell is hodmadod.It is described silane coupled
Agent is silane resin acceptor kh-550.
Example 2
Animal shell is placed in ball mill, under the conditions of rotating speed is 600r/min, ball mill grinding, the sieve of 300 mesh is crossed, obtains crust
Particle；By the hydrochloric acid in mass ratio 1 that gained crust particle and mass fraction are 10%：100 are added in No. 3 beakers, then No. 3 are burnt
Cup moves to digital display and tested the speed in constant temperature blender with magnetic force, is 80 DEG C in temperature, under the conditions of rotating speed is 400r/min, is stirred
After 30min, filtering, acid treatment filter residue is produced；Gained acid treatment filter residue and mass fraction are pressed into matter for 20% sodium hydroxide solution
Measure ratio 1：100 add in three-necked flasks, and three-necked flask then is moved into digital display tests the speed in constant temperature blender with magnetic force, in temperature be 80
DEG C, under the conditions of rotating speed is 400r/min, 40min is stirred, then burnt with 2.5mL/min speed to three mouthfuls with constant pressure funnel
The hydrochloric acid that mass fraction is 10% is added dropwise in bottle, regulation pH is 7.3, after the hydrochloric acid solution that mass fraction is 10% is added dropwise,
Filtering, obtains pretreated material, then pretreated material is washed with deionized 5 times, produces filter cake；By gained filter cake with it is anhydrous
Ethanol in mass ratio 1：100 are added in four-hole boiling flasks, then four-hole boiling flask is moved into digital display and tested the speed in constant temperature blender with magnetic force, Yu Wen
Spend for 85 DEG C, under the conditions of rotating speed is 400r/min, after heating stirring backflow 50min, filtering, obtains filtrate, gained filtrate is placed in
It it is 85 DEG C, pressure 400kPa in temperature, under the conditions of rotating speed is 80r/min, be concentrated under reduced pressure 20min, produces in Rotary Evaporators
Crust extract solution；Count in parts by weight, by 40 parts of silica flours, 40 parts of sodium hydroxide solutions, 120 parts of water, 20 parts of reaction products, 20 parts
Crust extract solution, 20 parts of silane couplers are added in batch mixer, added in No. 4 beakers, under the conditions of rotating speed is 500r/min, are stirred
Hybrid reaction 50min is mixed, produces mixed slurry；Gained mixed slurry is placed in press filtration 30min in filter press, obtains press filtration slurry,
Then gained press filtration slurry is placed in Rotary Evaporators, is 110 DEG C, pressure 400kPa in temperature, rotating speed is 90r/min bars
Under part, be concentrated under reduced pressure 30min, is concentrated under reduced pressure, and produces industry silicasol.The animal shell is hodmadod.It is described silane coupled
Agent is silane resin acceptor kh-550.
Example 3
By pigskin and water in mass ratio 1：30 add in No. 1 beaker, stir 20min with glass bar, then No. 1 beaker is placed in into refrigerator
Middle freezing 3h, obtains frozen block；Gained frozen block is placed in freezing crusher, crushed, the sieve of 100 mesh is crossed, produces crushed material；Will
Gained crushed material is placed in No. 2 beakers, and No. 2 beakers are moved into digital display tests the speed in constant temperature blender with magnetic force, is 80 DEG C in temperature, is turned
Under the conditions of speed is 400r/min, heating stirring is melted to complete, is obtained thawing solution, is then filtered thawing solution, obtains wet stock, then will
Wet stock, which is placed in vacuum freezing drying oven, dries 50min, obtains filter residue；Filter residue and mass fraction are pressed into quality for 10% sulfuric acid
1：10 mixing after, be placed in crucible, in temperature be 140 DEG C under the conditions of, and use glass bar stirring reaction 40min, produce reaction produce
Thing；Count in parts by weight, by 40 parts of silica flours, 40 parts of sodium hydroxide solutions, 120 parts of water, 20 parts of reaction products, 20 parts of crust extractions
Liquid, 20 parts of silane couplers are added in batch mixer, added in No. 4 beakers, under the conditions of rotating speed is 500r/min, are stirred anti-
50min is answered, produces mixed slurry；Gained mixed slurry is placed in press filtration 30min in filter press, obtains press filtration slurry, then by institute
Obtain press filtration slurry to be placed in Rotary Evaporators, be 110 DEG C, pressure 400kPa in temperature, under the conditions of rotating speed is 90r/min, subtract
Pressure concentration 30min, is concentrated under reduced pressure, produces industry silicasol.The animal shell is hodmadod.The silane coupler is silane
Coupling agent KH-550.
Comparative example：The Ludox of Hubei Science and Technology Ltd. production.
The gained of example 1 to 3 Ludox and comparative example product are subjected to performance detection, specific detection method is as follows：
Pencil hardness：Organic-silicon-modified Ludox is coated on steel plate, after 200 DEG C of solidification 1h, QFZ type lead is used by GB/T6739
Hardometer is tested.
Film adhesive：Organic-silicon-modified Ludox is coated on steel plate, after 200 DEG C of solidification 1h, used by GB/T9286
PPH-I type paint film adhesions instrument is tested.
Specific testing result is as shown in table 1：
Table 1
| Detection content | Example 1 | Example 2 | Example 3 | Comparative example |
| Solidify result | Surface flawless | Surface flawless | Surface flawless | There is crackle on surface |
| Hardness | 7H | 6H | 6H | 5H |
| Adhesive force/level | 0 | 1 | 1 | 2 |
From the testing result of table 1, industry silicasol provided by the invention has excellent performance, is effectively prevented from Ludox shape
Into membrane rigidity it is big, be easily cracked, the problem of gloss difference.
Claims (5)
1. a kind of preparation method of industry silicasol, it is characterised in that specifically preparation process is：
（1）By pigskin and water in mass ratio 1：20~1：After being mixed in 30 No. 1 beakers of addition, it is placed in refrigerator and freezes, must freeze
Block；
（2）Above-mentioned gained frozen block is placed in freezing crusher, crushed, sieving, produces crushed material；
（3）Above-mentioned gained crushed material is placed in No. 2 beakers, dissolved by heating, is filtered, dries, obtains filter residue；
（4）It is 1 in mass ratio by filter residue and sulfuric acid：5~1：After 10 mixing, it is placed in crucible, heating stirring reaction, production must be reacted
Thing；
（5）Animal shell is placed in ball mill, ball mill grinding, sieves, obtain crust particle；
（6）By above-mentioned gained crust particle and hydrochloric acid in mass ratio 1：50~1：100 add in No. 3 beakers, heating stirring mixing,
Filtering, produces acid treatment filter residue；
（7）By above-mentioned gained acid treatment filter residue and sodium hydroxide solution in mass ratio 1：50~1：100 add in three-necked flask, add
Thermal agitation mixes, then salt acid for adjusting pH is added dropwise, and filters, and washing, produces filter cake；
（8）By above-mentioned gained filter cake and ethanol in mass ratio 1：50~1：100 add in four-hole boiling flask, heating stirring backflow, mistake
Filter, is concentrated under reduced pressure, produces crust extract solution；
（9）Count in parts by weight, by 30~40 parts of silica flours, 30~40 parts of sodium hydroxide solutions, 100~120 parts of water, 10~20 parts
Reaction product, 10~20 parts of crust extract solutions, 10~20 parts of silane coupler mixing, stirring reaction, produce mixed slurry；
（10）By above-mentioned gained mixed slurry press filtration, it is concentrated under reduced pressure, produces industry silicasol.
A kind of 2. preparation method of industry silicasol according to claim 1, it is characterised in that：Step（2）It is described to cross sieve mesh
Number is the sieve of 80~100 mesh.
A kind of 3. preparation method of industry silicasol according to claim 1, it is characterised in that：Step（5）The animal first
Shell is hodmadod, any one in snail shell or freshwater mussel shell.
A kind of 4. preparation method of industry silicasol according to claim 1, it is characterised in that：Step（5）It is described to cross sieve mesh
Number is the sieve of 200~300 mesh.
A kind of 5. preparation method of industry silicasol according to claim 1, it is characterised in that：Step（9）The silane is even
Connection agent is silane resin acceptor kh-550, any one in silane coupler KH-560 or Silane coupling reagent KH-570.
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| CN201710933591.1A CN107551963A (en) | 2017-10-10 | 2017-10-10 | A kind of preparation method of industry silicasol |
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| CN201710933591.1A CN107551963A (en) | 2017-10-10 | 2017-10-10 | A kind of preparation method of industry silicasol |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974385A (en) * | 2006-12-08 | 2007-06-06 | 中国科学院宁波材料技术与工程研究所 | Prepn process of monodispersive silica sol |
| CN102040868A (en) * | 2010-11-24 | 2011-05-04 | 上海迪升防腐新材料科技有限公司 | Method for preparation and surface modification of alkaline silicon sol |
| CN105288734A (en) * | 2015-11-23 | 2016-02-03 | 四川大学 | Composite crosslinked type I collagen membrane and preparation method thereof |
| CN106479307A (en) * | 2016-10-14 | 2017-03-08 | 宁波市鄞州煜隆工具有限公司 | Metal tube and preparation method thereof |
| CN106927465A (en) * | 2015-12-31 | 2017-07-07 | 江苏天恒纳米科技股份有限公司 | A kind of preparation method of modified Nano silica flour |
-
2017
- 2017-10-10 CN CN201710933591.1A patent/CN107551963A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974385A (en) * | 2006-12-08 | 2007-06-06 | 中国科学院宁波材料技术与工程研究所 | Prepn process of monodispersive silica sol |
| CN102040868A (en) * | 2010-11-24 | 2011-05-04 | 上海迪升防腐新材料科技有限公司 | Method for preparation and surface modification of alkaline silicon sol |
| CN105288734A (en) * | 2015-11-23 | 2016-02-03 | 四川大学 | Composite crosslinked type I collagen membrane and preparation method thereof |
| CN106927465A (en) * | 2015-12-31 | 2017-07-07 | 江苏天恒纳米科技股份有限公司 | A kind of preparation method of modified Nano silica flour |
| CN106479307A (en) * | 2016-10-14 | 2017-03-08 | 宁波市鄞州煜隆工具有限公司 | Metal tube and preparation method thereof |
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