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 PDF

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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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temperature
reaction
thixotropic agent
beaker
temperature resistant
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赵玲玲
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Jiangsu Tuo Tuo Electric Technology Co Ltd
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Jiangsu Tuo Tuo Electric Technology Co Ltd
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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

A kind of preparation method of high temperature resistant thixotropic agent
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.
CN201910079748.8A 2019-01-28 2019-01-28 A kind of preparation method of high temperature resistant thixotropic agent Pending CN109704610A (en)

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