CN109704610A - A kind of preparation method of high temperature resistant thixotropic agent - Google Patents
A kind of preparation method of high temperature resistant thixotropic agent Download PDFInfo
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- CN109704610A CN109704610A CN201910079748.8A CN201910079748A CN109704610A CN 109704610 A CN109704610 A CN 109704610A CN 201910079748 A CN201910079748 A CN 201910079748A CN 109704610 A CN109704610 A CN 109704610A
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- thixotropic agent
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- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 43
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 20
- 241000609240 Ambelania acida Species 0.000 claims abstract description 14
- 240000005158 Phaseolus vulgaris Species 0.000 claims abstract description 14
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims abstract description 14
- 239000010905 bagasse Substances 0.000 claims abstract description 14
- WQZGKKKJIJFFOK-GASJEMHNSA-N D-Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 12
- 239000008103 glucose Substances 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 11
- 239000000047 product Substances 0.000 claims description 33
- 239000007795 chemical reaction product Substances 0.000 claims description 24
- 238000000227 grinding Methods 0.000 claims description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 21
- 238000009835 boiling Methods 0.000 claims description 20
- 241000218628 Ginkgo Species 0.000 claims description 18
- 235000011201 Ginkgo Nutrition 0.000 claims description 18
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L MgCl2 Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 18
- VZJVWSHVAAUDKD-UHFFFAOYSA-N Potassium permanganate Chemical compound [K+].[O-][Mn](=O)(=O)=O VZJVWSHVAAUDKD-UHFFFAOYSA-N 0.000 claims description 18
- 235000000381 ginkgo Nutrition 0.000 claims description 18
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 16
- 230000001264 neutralization Effects 0.000 claims description 16
- 210000002966 Serum Anatomy 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- UIIMBOGNXHQVGW-UHFFFAOYSA-M NaHCO3 Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-Butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 6
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 238000007792 addition Methods 0.000 claims description 4
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims 1
- 239000004568 cement Substances 0.000 abstract description 13
- 239000004567 concrete Substances 0.000 abstract description 9
- 239000005416 organic matter Substances 0.000 abstract description 9
- RGHNJXZEOKUKBD-SQOUGZDYSA-N Gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 abstract description 8
- 239000000835 fiber Substances 0.000 abstract description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract description 8
- 238000010008 shearing Methods 0.000 abstract description 8
- JLVVSXFLKOJNIY-UHFFFAOYSA-N magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 abstract description 6
- 229910001425 magnesium ion Inorganic materials 0.000 abstract description 6
- CZMRCDWAGMRECN-UGDNZRGBSA-N D-sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 abstract description 5
- CZMRCDWAGMRECN-GDQSFJPYSA-N Sucrose Natural products O([C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O1)[C@@]1(CO)[C@H](O)[C@@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-GDQSFJPYSA-N 0.000 abstract description 5
- 102000004169 proteins and genes Human genes 0.000 abstract description 5
- 108090000623 proteins and genes Proteins 0.000 abstract description 5
- 239000005720 sucrose Substances 0.000 abstract description 5
- 239000000654 additive Substances 0.000 abstract description 4
- 239000000174 gluconic acid Substances 0.000 abstract description 4
- 235000012208 gluconic acid Nutrition 0.000 abstract description 4
- 229950006191 gluconic acid Drugs 0.000 abstract description 4
- 239000000395 magnesium oxide Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000001913 cellulose Substances 0.000 abstract description 3
- 229920002678 cellulose Polymers 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 150000004676 glycans Polymers 0.000 abstract description 3
- 239000004615 ingredient Substances 0.000 abstract description 3
- 229920001282 polysaccharide Polymers 0.000 abstract description 3
- 239000005017 polysaccharide Substances 0.000 abstract description 3
- 150000004804 polysaccharides Polymers 0.000 abstract description 3
- 229920002488 Hemicellulose Polymers 0.000 abstract description 2
- 230000000536 complexating Effects 0.000 abstract description 2
- 229920001184 polypeptide Polymers 0.000 abstract description 2
- 239000000284 extract Substances 0.000 abstract 1
- 235000011121 sodium hydroxide Nutrition 0.000 abstract 1
- 239000002002 slurry Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 230000003247 decreasing Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920002401 polyacrylamide Polymers 0.000 description 2
- 239000003638 reducing agent Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2R,3R,4S,5R,6S)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2S,3R,4S,5R,6R)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2R,3R,4S,5R,6R)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 description 1
- 239000004382 Amylase Substances 0.000 description 1
- 102000013142 Amylases Human genes 0.000 description 1
- 108010065511 Amylases Proteins 0.000 description 1
- 102000033147 ERVK-25 Human genes 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 206010018987 Haemorrhage Diseases 0.000 description 1
- 230000036740 Metabolism Effects 0.000 description 1
- 108091005771 Peptidases Proteins 0.000 description 1
- 229920001231 Polysaccharide peptide Polymers 0.000 description 1
- 239000004365 Protease Substances 0.000 description 1
- 229920002310 Welan gum Polymers 0.000 description 1
- 230000000996 additive Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000019418 amylase Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000740 bleeding Effects 0.000 description 1
- 231100000319 bleeding Toxicity 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000004059 degradation Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
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- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000001050 lubricating Effects 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 230000035786 metabolism Effects 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
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- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000002441 reversible Effects 0.000 description 1
- 238000007665 sagging Methods 0.000 description 1
- 239000011376 self-consolidating concrete Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 230000003313 weakening Effects 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N β-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
Abstract
The present invention relates to a kind of preparation methods of high temperature resistant thixotropic agent, belong to technical field of concrete additives.The present invention utilizes acid soak, high-temperature high-voltage reaction extracts from bagasse and bean dregs and obtains cellulose, hemicellulose, sucrose, the ingredients such as protein, sucrose simultaneously, protein portion, which decomposes, generates glucose, the substances such as the shorter polysaccharide of chain length and polypeptide, corrosion of the fiber molecule extracted from bean dregs and bagasse by high-temperature high-voltage reaction and acid solution, form fracture, molecular chain length greatly reduces, advantageous thixotropic agent network structure when by shearing force is more easier to be destroyed, magnesium ion is introduced into gluconic acid and fiber molecule, utilize wherein carboxylic group absorption complexing magnesium ion abundant, fall to magnesium ion in organic matter, to with after lye pyroreaction, in organic matter surface growing nano grade magnesia, magnesia covered section organic matter, to protect organic matter to prevent from being thermally decomposed, reinforce cement Rigidity and mechanical strength.
Description
Technical field
The present invention relates to a kind of preparation methods of high temperature resistant thixotropic agent, belong to technical field of concrete additives.
Background technique
When lubricating grease is sheared, consistency becomes smaller, and when stopping shearing, increased property is thixotropy to consistency again.Thixotroping
Property also known as shake change.It is the reversible colloidal sol phenomenon that gelinite occurs under the action of the mechanical forces such as oscillation, compressing.It is by not sieve
Because of Freundlich discovery.Elongated particle links to form reticular structure by weak chemical bond, it is easy to be destroyed by external force, answer extensively
For building, coating industry.Also known as anti-sag agent and anti-sagging agent.
Thixotropic agent is a kind of novel cement concrete admixture researched and developed in recent years, adds the mesh of this additive
Be increase the cohesiveness and cohesive force of cement cementitious material, reduce the separation rate of material component, improve homogeneity and hardening
The performance of product.Thixotropic cement slurry system is mainly made of cement and thixotropic agent, and the key of preparation thixotroping cement is thixotropic agent
Selection and reasonable employment.The mechanism of action of thixotropic agent are as follows: thixotropic agent is capable of forming network knot in cement slurry or concrete
Structure is formed by network structure and is destroyed when system is by shearing force, and system restores mobility, and viscosity reduces；Work as shearing force
When stopping, system re-forms network structure, and viscosity increases.
Usually in prestressed grouting, self-leveling concrete, self-compacting concrete, not high flowabilities such as discrete concrete under water
Thixotropic agent is added in system, is on the one hand the rheological characteristic for improving concrete using it, reduces the viscosity of concrete agitation phases；Separately
On the one hand the yield stress that system is improved using it, to improve limit doped amount of the water-reducing agent in cement-based systems, solve because
Bleeding problem is isolated caused by water-reducing agent excess.
Common thixotropic agent has, cellulose water soluble polymer, polyacrylamide, biogum, glucose or sucrose etc.
High polymer, wherein at most with the application of cellulose ether, methylcellulose, polyacrylamide, xanthan gum, welan gum etc., but at present
These existing thixotropic agent are there are volume height, and thixotropic property is general, and thixotropy is not strong enough, so that its work cannot be played effectively
With；It is temperature sensitive；Thixotropy is preferable under room temperature, but as the temperature rises, thixotropy is decreased obviously；Comprehensive performance is not good enough.
Therefore, the thixotropic agent that a kind of thixotropic property is good and high temperature resistance is good is invented to have technical field of concrete additives
There is positive effect.
Summary of the invention
The technical problems to be solved by the invention: it is insufficient for current thixotropic agent thixotropic property, as temperature improves thixotroping
The defect of performance decline, provides a kind of preparation method of high temperature resistant thixotropic agent.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of high temperature resistant thixotropic agent the preparation method comprises the following steps:
Tunning is put into beaker, is placed the beaker in the water-bath that bath temperature is 90~100 DEG C, constant temperature boiling 100
The sodium hydroxide solution that mass fraction is 12~14% is added dropwise into beaker and adjusts pH value to 11~12, continues constant temperature by~120min
2~3h of boiling, the salt acid for adjusting pH value that dropwise addition mass fraction is 10~12% after boiling to neutrality；
It places the beaker in vacuum oven, stands 12 under conditions of vacuum degree is 120~160Pa and temperature is 30~36 DEG C
Desciccate is made in~14h, desciccate and butyl glycol ether is put into beaker, with agitating device with 400~500r/min
Revolving speed be mixed 50~70min, material is concentrated into the 55~65% of original volume to get high temperature resistant thixotropic agent after stirring；
Tunning the preparation method comprises the following steps:
The sodium bicarbonate solution that mass fraction is 6~10% is added dropwise into reaction kettle and adjusts modified-reaction product pH value to neutrality system
Neutral products, will neutral products, ginkgo leaf, ginkgo tree root investment pulverizer in crush be blended be made mixture, according to
Secondary acetone and washes of absolute alcohol mixture 3~5 times, mixture is putted into fermenter with glucose and is uniformly mixed, will be upper
It states fermentor to be placed in the greenhouse that ambient temperature is 32~36 DEG C, opening stands 8~10 days obtained tunnings；
Modified-reaction product the preparation method comprises the following steps:
(1) bagasse is mixed with bean dregs in investment baking oven, dry 10~12h, dry under conditions of temperature is 70~80 DEG C
It puts into planetary ball mill afterwards, 2~3h is ground under conditions of ratio of grinding media to material is 5:1 and revolving speed is 300~360r/min and crosses 50 mesh
Sieve obtains grinding product；
(2) it by grinding product and hydrochloric acid investment beaker, places the beaker in sonic oscillation instrument, is 36~40kHz's in frequency
Under the conditions of 4~6h of oscillation mixed serum is made, by mixed serum and magnesium chloride investment reaction kettle, with agitating device with 400~
30~40min is mixed in the revolving speed of 500r/min；
(3) reactor temperature is increased to 110~120 DEG C, pyrohydrolysis liquid is made in 2~3h of isothermal reaction, into reaction kettle
Potassium permanganate is added, 30~40min is mixed with the revolving speed of 800~900r/min with blender, oxidation solution is made, will reacted
Kettle is closed, and nitrogen is filled with into reaction kettle, and increasing air pressure in kettle, to 1.4~1.8MPa, constant pressure, which stands 80~100min and is made, to be changed
Property reaction product.
The mass ratio of desciccate and butyl glycol ether is 2:3.
In the preparation method of tunning according to parts by weight: neutral products are 20~22 parts, ginkgo leaf is 1~2
Part, ginkgo tree root are 2~3 parts.
The mass ratio of mixture and glucose is 20:1 in the preparation method of tunning.
The mass ratio of bagasse and bean dregs is 4:1 in the preparation method of modified-reaction product.
The mass ratio of grinding product and hydrochloric acid is 1:10 in the preparation method of modified-reaction product, and the mass fraction of hydrochloric acid is
8~12%.
The mass ratio of mixed serum and magnesium chloride is 20:1 in the preparation method of modified-reaction product.
The quality of potassium permanganate is the 3~5% of pyrohydrolysis liquid quality in the preparation method of modified-reaction product.
The method have the benefit that:
(1) bean dregs and bagasse combination drying are ground grinding product is made first by the present invention, then by grinding product and hydrochloric acid
Mixing is added magnesium chloride and is mixed after mixing, pyroreaction after stirring adds potassium permanganate oxidation, and high temperature is high after oxidation
Pressure, which is reacted, is made neutral products, is then blended with ginkgo leaf, tree root crushing, then puts into fermenter hair neutral products
Ferment, after fermentation adjust pH value to alkalinity after high temperature boiling, after boiling be concentrated and dried be made desciccate, finally by desciccate with
Butyl glycol ether is mixed, and is discharged after concentration up to high temperature resistant thixotropic agent, the present invention utilizes acid soak, high-temperature high-voltage reaction
It is extracted from bagasse and bean dregs and obtains the ingredients such as cellulose, hemicellulose, sucrose, protein, while sucrose, protein portion
It decomposes and generates substances, glucose and the polysaccharide molecules such as glucose, chain length shorter polysaccharide and polypeptide through excessively high manganese
Sour potassium oxidation, surface hydroxyl reaction generate carboxyl, form gluconic acid and polyvalent carboxylic ingredient, so that it is viscous to be conducive to reinforcement absorption
Fiber molecule, while corrosion of the fiber molecule extracted from bean dregs and bagasse by high-temperature high-voltage reaction and acid solution are tied,
Organic molecule chain is caused to be broken, molecular chain length greatly reduces, and network structure is more when by shearing force to be conducive to thixotropic agent
Add and be more easily damaged, and is easy to adsorbing fiber molecular recombination network knot after shearing force disappearance using gluconic acid and polysaccharide acid
Structure, to improve the thixotropic property of thixotropic agent；
(2) magnesium ion is introduced into gluconic acid and fiber molecule by the present invention, utilization wherein carboxylic group absorption complexing abundant
Magnesium ion falls to magnesium ion in organic matter, then react respectively with alkali and pyroreaction after, on organic matter surface, growth is received
Meter level magnesia, magnesia covered section organic matter fill the pore structure between organic matter, make thixotropic agent in cement solidification
The network structure of formation is stronger, hard, so that organic matter be protected to prevent from being thermally decomposed, avoids weakening thixotropic property, and add
The rigidity and mechanical strength of strong cement, the present invention also utilize ginkgo leaf, the endophyte growth metabolism in tree root to generate fiber
The substances such as plain enzyme, amylase, protease carry out organic fiber, carbohydrate molecule, the protein molecule in bean dregs, bagasse
Further degradation, and carboxylic acid corrosion metal ion is generated, keep metal ion dispersion more uniform, increases organo-functional group quantity
To increase bonding force quantity, the compactness and stability of the micro-space structure after improving cement solidification process have wide
Application prospect.
Specific embodiment
Bagasse is mixed in investment baking oven with bean dregs 4:1 in mass ratio, it is dry under conditions of temperature is 70~80 DEG C
10~12h puts into planetary ball mill after dry, grinds under conditions of ratio of grinding media to material is 5:1 and revolving speed is 300~360r/min
2~3h crosses 50 meshes and obtains grinding product；The hydrochloric acid 1:10 in mass ratio that grinding product and mass fraction are 8~12% is put into
In beaker, placing the beaker in sonic oscillation instrument, mixed serum is made in 4~6h of oscillation under conditions of frequency is 36~40kHz,
By in mixed serum and magnesium chloride 20:1 in mass ratio investment reaction kettle, mixed with agitating device with the revolving speed of 400~500r/min
Close 30~40min of stirring；Temperature in aforesaid reaction vessel is increased to 110~120 DEG C, pyrohydrolysis is made in 2~3h of isothermal reaction
Liquid the potassium permanganate of pyrohydrolysis liquid quality 3~5% is added into reaction kettle, with blender with the revolving speed of 800~900r/min
30~40min is mixed, oxidation solution is made, reaction kettle is closed, it is filled with nitrogen into reaction kettle, increases in kettle air pressure to 1.4
~1.8MPa, constant pressure stand 80~100min and modified-reaction product are made；Into aforesaid reaction vessel be added dropwise mass fraction be 6~
10% sodium bicarbonate solution adjusts modified-reaction product pH value to the obtained neutral products of neutrality, according to parts by weight, by 20~22
Part neutral products, 1~2 part of ginkgo leaf, 2~3 parts of ginkgo tree roots, which put into pulverizers to crush to be blended, is made mixture, according to
Secondary acetone and washes of absolute alcohol mixture 3~5 times, mixture are putted into fermenter with glucose 20:1 in mass ratio mixed
It closes uniformly, fermentor is placed in the greenhouse that ambient temperature is 32~36 DEG C, opening stands 8~10 days obtained tunnings；It will
In above-mentioned tunning investment beaker, place the beaker in the water-bath that bath temperature is 90~100 DEG C, constant temperature boiling 100~
The sodium hydroxide solution that mass fraction is 12~14% is added dropwise into beaker and adjusts pH value to 11~12, continues thermostatted water by 120min
2~3h is boiled, the salt acid for adjusting pH value that dropwise addition mass fraction is 10~12% after boiling to neutrality；Above-mentioned beaker is placed in vacuum to do
In dry case, 12~14h is stood under conditions of vacuum degree is 120~160Pa and temperature is 30~36 DEG C, desciccate is made, it will
In desciccate and butyl glycol ether 2:3 in mass ratio investment beaker, mixed with agitating device with the revolving speed of 400~500r/min
50~70min is stirred, material is concentrated into the 55~65% of original volume to get high temperature resistant thixotropic agent after stirring.
Example 1
The preparation of modified-reaction product:
Bagasse is mixed in investment baking oven with bean dregs 4:1 in mass ratio, dry 10h, dry under conditions of temperature is 70 DEG C
It puts into planetary ball mill afterwards, grinding 2h crosses 50 meshes and ground under conditions of ratio of grinding media to material is 5:1 and revolving speed is 300r/min
Grind product；
The hydrochloric acid 1:10 in mass ratio that grinding product and mass fraction are 8% is put into beaker, sonic oscillation instrument is placed the beaker
In, mixed serum is made in oscillation 4h under conditions of frequency is 36kHz, and mixed serum and magnesium chloride 20:1 in mass ratio are put into
In reaction kettle, 30min is mixed with the revolving speed of 400r/min with agitating device；
Temperature in aforesaid reaction vessel is increased to 110 DEG C, pyrohydrolysis liquid is made in isothermal reaction 2h, and high temperature is added into reaction kettle
The potassium permanganate of hydrolyzate quality 3% is mixed 30min with blender with the revolving speed of 800r/min and oxidation solution is made, will react
Kettle is closed, and nitrogen is filled with into reaction kettle, and increasing air pressure in kettle, to 1.4MPa, constant pressure stands the obtained modified-reaction product of 80min.
The preparation of tunning:
The sodium bicarbonate solution that mass fraction is 6% is added dropwise into aforesaid reaction vessel and adjusts modified-reaction product pH value to neutrality system
Neutral products are obtained, according to parts by weight, 20 parts of neutral products, 1 part of ginkgo leaf, 2 parts of ginkgo tree roots are put into pulverizers
Middle crushing, which is blended, is made mixture, and successively with acetone and washes of absolute alcohol mixture 3 times, mixture and glucose are pressed quality
Putted into fermenter than 20:1 uniformly mixed, it is in 32 DEG C of greenhouse that fermentor, which is placed in ambient temperature, and opening stands 8 days and is made
Tunning.
The preparation of high temperature resistant thixotropic agent:
Above-mentioned tunning is put into beaker, is placed the beaker in the water-bath that bath temperature is 90 DEG C, constant temperature boiling
The sodium hydroxide solution that mass fraction is 12% is added dropwise into beaker and adjusts pH value to 11, continues constant temperature boiling 2h, water by 100min
Salt acid for adjusting pH value that mass fraction is 10% is added dropwise after boiling to neutrality；
Above-mentioned beaker is placed in a vacuum drying oven, 12h is stood under conditions of vacuum degree is 120Pa and temperature is 30 DEG C and is made
Desciccate puts into desciccate and butyl glycol ether 2:3 in mass ratio in beaker, with agitating device turning with 400r/min
50min is mixed in speed, and material is concentrated into the 55% of original volume to get high temperature resistant thixotropic agent after stirring.
Example 2
The preparation of modified-reaction product:
Bagasse is mixed in investment baking oven with bean dregs 4:1 in mass ratio, dry 11h, dry under conditions of temperature is 75 DEG C
It puts into planetary ball mill afterwards, grinding 2.5h crosses 50 meshes and obtains under conditions of ratio of grinding media to material is 5:1 and revolving speed is 350r/min
Grinding product；
The hydrochloric acid 1:10 in mass ratio that grinding product and mass fraction are 10% is put into beaker, sonic oscillation is placed the beaker
In instrument, mixed serum is made in oscillation 5h under conditions of frequency is 38kHz, and mixed serum and magnesium chloride 20:1 in mass ratio are thrown
Enter in reaction kettle, 35min is mixed with the revolving speed of 450r/min with agitating device；
Temperature in aforesaid reaction vessel is increased to 115 DEG C, pyrohydrolysis liquid is made in isothermal reaction 2.5h, is added into reaction kettle high
The potassium permanganate of warm hydrolyzate quality 4% is mixed 35min with blender with the revolving speed of 850r/min and oxidation solution is made, will be anti-
It answers kettle closed, nitrogen is filled with into reaction kettle, increasing air pressure in kettle, to 1.6MPa, constant pressure stands 90min and modified-reaction production is made
Object.
The preparation of tunning:
The sodium bicarbonate solution that mass fraction is 8% is added dropwise into aforesaid reaction vessel and adjusts modified-reaction product pH value to neutrality system
Neutral products are obtained, according to parts by weight, 21 parts of neutral products, 1 part of ginkgo leaf, 2 parts of ginkgo tree roots are put into pulverizers
Middle crushing, which is blended, is made mixture, and successively with acetone and washes of absolute alcohol mixture 4 times, mixture and glucose are pressed quality
Putted into fermenter than 20:1 uniformly mixed, it is in 34 DEG C of greenhouse that fermentor, which is placed in ambient temperature, and opening stands 9 days and is made
Tunning.
The preparation of high temperature resistant thixotropic agent:
Above-mentioned tunning is put into beaker, is placed the beaker in the water-bath that bath temperature is 95 DEG C, constant temperature boiling
1100min, the sodium hydroxide solution adjusting pH value that dropwise addition mass fraction is 13% into beaker to 11, continues constant temperature boiling 2.5h,
Salt acid for adjusting pH value that mass fraction is 11% is added dropwise after boiling to neutrality；
Above-mentioned beaker is placed in a vacuum drying oven, 13h is stood under conditions of vacuum degree is 140Pa and temperature is 33 DEG C and is made
Desciccate puts into desciccate and butyl glycol ether 2:3 in mass ratio in beaker, with agitating device turning with 450r/min
60min is mixed in speed, and material is concentrated into the 60% of original volume to get high temperature resistant thixotropic agent after stirring.
Example 3
The preparation of modified-reaction product:
Bagasse is mixed in investment baking oven with bean dregs 4:1 in mass ratio, dry 12h, dry under conditions of temperature is 80 DEG C
It puts into planetary ball mill afterwards, grinding 3h crosses 50 meshes and ground under conditions of ratio of grinding media to material is 5:1 and revolving speed is 360r/min
Grind product；
The hydrochloric acid 1:10 in mass ratio that grinding product and mass fraction are 12% is put into beaker, sonic oscillation is placed the beaker
In instrument, mixed serum is made in oscillation 6h under conditions of frequency is 40kHz, and mixed serum and magnesium chloride 20:1 in mass ratio are thrown
Enter in reaction kettle, 40min is mixed with the revolving speed of 500r/min with agitating device；
Temperature in aforesaid reaction vessel is increased to 120 DEG C, pyrohydrolysis liquid is made in isothermal reaction 3h, and high temperature is added into reaction kettle
The potassium permanganate of hydrolyzate quality 5% is mixed 40min with blender with the revolving speed of 900r/min and oxidation solution is made, will react
Kettle is closed, and nitrogen is filled with into reaction kettle, and increasing air pressure in kettle, to 1.8MPa, constant pressure stands 100min and modified-reaction production is made
Object.
The preparation of tunning:
The sodium bicarbonate solution that mass fraction is 10% is added dropwise into aforesaid reaction vessel and adjusts modified-reaction product pH value to neutrality system
Neutral products are obtained, according to parts by weight, 22 parts of neutral products, 2 parts of ginkgo leaves, 3 parts of ginkgo tree roots are put into pulverizers
Middle crushing, which is blended, is made mixture, and successively with acetone and washes of absolute alcohol mixture 5 times, mixture and glucose are pressed quality
Putted into fermenter than 20:1 uniformly mixed, it is in 36 DEG C of greenhouse that fermentor, which is placed in ambient temperature, and opening stands 10 days and makes
Obtain tunning.
The preparation of high temperature resistant thixotropic agent:
Above-mentioned tunning is put into beaker, is placed the beaker in the water-bath that bath temperature is 100 DEG C, constant temperature boiling
The sodium hydroxide solution that mass fraction is 14% is added dropwise into beaker and adjusts pH value to 12, continues constant temperature boiling 3h, water by 120min
Salt acid for adjusting pH value that mass fraction is 12% is added dropwise after boiling to neutrality；
Above-mentioned beaker is placed in a vacuum drying oven, 14h is stood under conditions of vacuum degree is 160Pa and temperature is 36 DEG C and is made
Desciccate puts into desciccate and butyl glycol ether 2:3 in mass ratio in beaker, with agitating device turning with 500r/min
70min is mixed in speed, and material is concentrated into the 65% of original volume to get high temperature resistant thixotropic agent after stirring.
Comparative example 1: it is essentially identical with the preparation method of example 2, it has only the difference is that lacking modified-reaction product.
Comparative example 2: it is essentially identical with the preparation method of example 2, it has only the difference is that lacking tunning.
Comparative example 3: the high temperature resistant thixotropic agent of Shanghai company production.
Thixotropy test: machine is tested out using CM10 type torquemeter respectively, stands slurry after 15min, 30min and 60min
Determine torsion, after testing, slurry is stirred into 1min in blender, test, which is stood, determines torsion after 2min and 15min.The reality
The purpose tested is that slurry goes out machine standing and to stand again after shearing force destruction slurry, torque changes with time for observing
Gesture.
If slurry goes out machine standing, torque increases with the extension of time of repose, then tends towards stability, after being subject to shearing force,
Slurry restores flow-like, and torque is remarkably decreased, and illustrates that the slurry has good thixotropy, i.e. thixotropic agent performance is excellent.
Strength of cement test is detected by GB/T17671 standard.
1 thixotropic agent performance measurement result of table
Splendid according to above-mentioned detection data high temperature resistant thixotropic agent thixotropic property produced by the present invention, torque is with time of repose
Extend and increase, and heat resistance is good, reinforces the rigidity and mechanical strength of cement, has broad application prospects.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of high temperature resistant thixotropic agent, it is characterised in that specific preparation step are as follows:
(1) tunning is put into beaker, is placed the beaker in the water-bath that bath temperature is 90~100 DEG C, constant temperature boiling
The sodium hydroxide solution that mass fraction is 12~14% is added dropwise into beaker and adjusts pH value to 11~12, continues by 100~120min
Constant temperature 2~3h of boiling, the salt acid for adjusting pH value that dropwise addition mass fraction is 10~12% after boiling to neutrality；
(2) it places the beaker in vacuum oven, it is quiet under conditions of vacuum degree is 120~160Pa and temperature is 30~36 DEG C
It sets 12~14h and desciccate is made, desciccate and butyl glycol ether are put into beaker, with agitating device with 400~500r/
50~70min is mixed in the revolving speed of min, and material is concentrated into the 55~65% of original volume to get high temperature resistant thixotroping after stirring
Agent；
The specific preparation step of the tunning are as follows:
The sodium bicarbonate solution that mass fraction is 6~10% is added dropwise into reaction kettle and adjusts modified-reaction product pH value to neutrality system
Neutral products, will neutral products, ginkgo leaf, ginkgo tree root investment pulverizer in crush be blended be made mixture, according to
Secondary acetone and washes of absolute alcohol mixture 3~5 times, mixture is putted into fermenter with glucose and is uniformly mixed, will be upper
It states fermentor to be placed in the greenhouse that ambient temperature is 32~36 DEG C, opening stands 8~10 days obtained tunnings；
The specific preparation step of the modified-reaction product are as follows:
(1) bagasse is mixed with bean dregs in investment baking oven, dry 10~12h, dry under conditions of temperature is 70~80 DEG C
It puts into planetary ball mill afterwards, 2~3h is ground under conditions of ratio of grinding media to material is 5:1 and revolving speed is 300~360r/min and crosses 50 mesh
Sieve obtains grinding product；
(2) it by grinding product and hydrochloric acid investment beaker, places the beaker in sonic oscillation instrument, is 36~40kHz's in frequency
Under the conditions of 4~6h of oscillation mixed serum is made, by mixed serum and magnesium chloride investment reaction kettle, with agitating device with 400~
30~40min is mixed in the revolving speed of 500r/min；
(3) reactor temperature is increased to 110~120 DEG C, pyrohydrolysis liquid is made in 2~3h of isothermal reaction, into reaction kettle
Potassium permanganate is added, 30~40min is mixed with the revolving speed of 800~900r/min with blender, oxidation solution is made, will reacted
Kettle is closed, and nitrogen is filled with into reaction kettle, and increasing air pressure in kettle, to 1.4~1.8MPa, constant pressure, which stands 80~100min and is made, to be changed
Property reaction product.
2. a kind of preparation method of high temperature resistant thixotropic agent according to claim 1, it is characterised in that: desciccate and second two
The mass ratio of alcohol butyl ether is 2:3.
3. a kind of preparation method of high temperature resistant thixotropic agent according to claim 1, it is characterised in that: tunning it is specific
In preparation step preferably according to parts by weight, the neutral products are 20~22 parts, ginkgo leaf is 1~2 part, ginkgo
Setting tree root is 2~3 parts.
4. a kind of preparation method of high temperature resistant thixotropic agent according to claim 1, it is characterised in that: tunning it is specific
The mass ratio of mixture described in preparation step and glucose is 20:1.
5. a kind of preparation method of high temperature resistant thixotropic agent according to claim 1, it is characterised in that: modified-reaction product
The mass ratio of bagasse described in specific preparation step (1) and bean dregs is 4:1.
6. a kind of preparation method of high temperature resistant thixotropic agent according to claim 1, it is characterised in that: modified-reaction product
The mass ratio of grinding product described in specific preparation step (2) and hydrochloric acid is 1:10, and the mass fraction of hydrochloric acid is 8~12%.
7. a kind of preparation method of high temperature resistant thixotropic agent according to claim 1, it is characterised in that: modified-reaction product
The mass ratio of mixed serum described in specific preparation step (2) and magnesium chloride is 20:1.
8. a kind of preparation method of high temperature resistant thixotropic agent according to claim 1, it is characterised in that: modified-reaction product
The quality of potassium permanganate described in specific preparation step (3) is the 3~5% of pyrohydrolysis liquid quality.
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