CN108130057A - A kind of preparation method of heat resistant type fluid loss additive - Google Patents
A kind of preparation method of heat resistant type fluid loss additive Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of heat resistant type fluid loss additive, belong to well treatment agent technical field.By both sexes sulfonated phenol formaldehyde resin and polyurethane dispersing liquid in mass ratio 3：2~3：1 is mixed in blender, and the modified graphene oxide of 0.2~0.3 times of both sexes sulfonated phenol formaldehyde resin quality and the dispersant of 0.06~0.12 times of both sexes sulfonated phenol formaldehyde resin quality are added in into blender, in temperature be 45~65 DEG C, after rotating speed is stirred 10~20min under conditions of being 250~300r/min, heat resistant type fluid loss additive is obtained.Heat resistant type fluid loss additive prepared by technical solution of the present invention has the characteristics that excellent filtration reduction and heat resistance.
Description
Technical field
The invention discloses a kind of preparation methods of heat resistant type fluid loss additive, belong to well treatment agent technical field.
Background technology
Oil field welldrilling mud main ingredient be as soil and water and various auxiliary chemicals additives.In continuous drilling well
The referred to as dehydration of the phenomenon that Cheng Zhong, water penetrates into stratum, unit interval fluid loss is excessive, can bring a series of adverse consequences：The borehole wall collapses
Collapse, hole diameter reduce and drilling fluid be thickened the problems such as, so as to cause the generation of the serious accidents such as bit freezing.Fluid loss additive contains and clay
The adsorption group of suction-operated and aquation group occurs, it can change the property of wall surface mud cake in well：Inorganic agent is adsorbed big
Clay particle surface forms layer protecting film, and subtle clay particle is adsorbed on big inorganic agent chain link, plays colloid protecting action,
Until as closely knit mud cake, the polar group of hydrone and chemical treatments（Aquation group）Or non-polar group and clay
Particle shape is into structural plane, and water, which will be bound in mud cake, to be passed through, and make permeability reduction, and reaching reduces water in drilling process
Effect to stratum leak-off.In order to reduce in drilling process water to stratum leak-off, ensure the suitable of well bore safety and drilling engineering
Profit carries out, and need to add in fluid loss additive.Common drilling well has with fluid loss additive：
1. sanlose and polyanion cellulose class, versatility is good, and filtrate reducing effect is good, and salt tolerant is strong.But heatproof
It is low, only 150 DEG C.Usage amount：0.5%~1.5%.
2. modified starch series：Mainly there are pregelatinized starch, carboxymethyl starch, hydroxyethyl starch, versatility is good, filtrate reducing effect
Fruit is good, and salt tolerant is strong.But heatproof is low, only 120 DEG C~140 DEG C.Usage amount：0.5%~1.5%.
3. sulfonation class：There is lignosulfonate to mix or be copolymerized with sulfonated-pheno-formoldehyde resin, sulfomethylation lignite and sulphur methyl
Phenolic resin mixing or copolymerization etc., filtrate reducing works well, and salt tolerant is strong, and temperature resistance is preferable.But usage amount is big, of high cost.It uses
Amount：1%~3%, dosage is slightly higher.
4. humic acid salts：Sodium humate, humic acid potassium, humic acid ferrochrome, nitre system humate etc., versatility is good, resists
Warm nature is preferable.But filtrate reducing effect is general, and usage amount is big, of high cost.Usage amount：1%~5%, dosage is higher.
5. copolymer analog and polyacrylate：By monomeric acrylic sodium, calcium acrylate, acrylamide, band sulfonic group and
Monomer difference composition with organic cationic groups, good combination property, temperature resistance are preferable.But have an impact to drilling fluid viscosity（Have
Thickening effect）, for low solids fluid, production cost is higher, and production technology is complicated.Usage amount：0.3%~1%.
Therefore, how to improve traditional fluid loss additive filtration reduction and the bad shortcoming of heat resistance, to obtain higher synthesis
The fluid loss additive of performance is that it is promoted and applies, meets industrial production demand urgent problem to be solved.
Invention content
The present invention solves the technical problem of：It is lacked for traditional fluid loss additive filtration reduction and heat resistance are bad
Point provides a kind of preparation method of heat resistant type fluid loss additive.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）By phenol and formaldehyde in mass ratio 3：2~4：2 mixing, after adjusting pH, are stirred to react, obtain mixed liquor, will
Mixed liquor and formaldehyde in mass ratio 8：1~8：2 mixing, and the sodium sulfite of 0.1~0.3 times of mixed liquor quality is sequentially added, it mixes
The dimethylamine of 0.2~0.3 times of liquid quality and the 1- bromobutane of 0.3~0.4 times of mixed liquor quality are closed, after being stirred, obtains both sexes
Sulfonated phenol formaldehyde resin blank washs both sexes sulfonated phenol formaldehyde resin blank 3~8 times, and by the both sexes sulfonated phenolic tree after washing
Fat blank and ethanol solution in mass ratio 1：5~1：10 mixing are impregnated, and are filtered, dry, obtain both sexes sulfonated phenol formaldehyde resin；
（2）By isoflurane chalcone diisocyanate and polypropylene glycol in mass ratio 1：1~2：1 mixing, and it is different to add in isophorone two
The dibutyl tin laurate that 0.1~0.2 times of cyanate quality obtains isoflurane chalcone diisocyanate mixed liquor, by isophorone
Diisocyanate mixed liquor heating stirring under nitrogen atmosphere is reacted, and obtains isoflurane chalcone diisocyanate reaction solution；
（3）By isoflurane chalcone diisocyanate reaction solution and dihydromethyl propionic acid in mass ratio 5：2~5：3 mixing, and add in different
The 1,4-butanediol of your 0.1~0.3 times of ketone di-isocyanate reaction liquid quality of fluorine, is stirred to react under nitrogen guard mode, obtains
Blank liquid is pre-processed, by pretreatment blank liquid cooling, and by the pretreatment blank liquid after cooling and silane coupling agent in mass ratio
3：1~3：2 mixing add in the acetone of 0.1~0.2 times of pretreatment blank liquid quality, are stirred under nitrogen atmosphere, obtain blank
Liquid, by blank liquid cool down after with triethylamine in mass ratio 5：1~5：2 mixing, spin concentration obtain polyurethane dispersing liquid；
（4）By both sexes sulfonated phenol formaldehyde resin and polyurethane dispersing liquid in mass ratio 3：2~3：1 mixing, and add in both sexes sulphonated phenol
The modified graphene oxide and the dispersion of 0.06~0.12 times of both sexes sulfonated phenol formaldehyde resin quality that 0.2~0.3 times of urea formaldehyde quality
Agent after being stirred, obtains heat resistant type fluid loss additive.
Step（3）The silane coupling agent is silane resin acceptor kh-550, silane coupling agent KH-560 or silane coupling agent
Any one in KH-570.
Step（4）The preparation method of the modified graphene oxide be by graphene oxide sonic oscillation, after centrifugation,
Concentrated by rotary evaporation, it is dry, pretreatment graphene oxide is obtained, by pretreatment graphene oxide with silane coupling agent KH-560 in mass ratio
1：3~1：5 mixing, and the water of 20~30 times of pretreatment graphene oxide quality is added in, after being stirred, filter, it is dry, it must change
Property graphene oxide
Step（4）The dispersant is Dispersant MF, any one in dispersant NNO or dispersant 5040.
The beneficial effects of the invention are as follows：
（1）The present invention adds in polyurethane dispersing liquid when preparing heat resistant type fluid loss additive, and first, the polyurethane dispersing liquid of addition can
Layer protecting film is generated on the argillic horizon formed during product use in the borehole wall, so as to which argillic horizon be made to be not easy to continue to thicken,
And then make product the filter loss of drilling fluid reduces in oil well after use, secondly, polyurethane molecular has in polyurethane dispersing liquid
Different grain sizes after adding in product, can be filled the hole in the borehole wall, so as to which product be made to bore in oil well after use
The filter loss of well liquid further reduces；
（2）The present invention adds in modified graphene oxide when preparing heat resistant type fluid loss additive, on the one hand, modified modified graphite oxide
Graphite is single chip architecture in alkene, after adding in product, can be combined during product use with the phenolic resin in system,
The clay layer surface that the borehole wall is formed forms one layer of graphene oxide protective film, make product after use in oil well drilling fluid leak-off
Amount reduces, on the other hand, since graphene oxide has preferable heat conductivility, so as to after adding in product, make the borehole wall
The heat conductivility for the film that surface is formed improves, and then improves the heat resistance of product.
Specific embodiment
By phenol and formaldehyde in mass ratio 3：2~4：2 are mixed in beaker, are 5~8% with mass fraction
Sodium hydroxide solution is adjusted in beaker after pH to 7~8, and beaker is moved into digital display constant temperature blender with magnetic force, in temperature be 90~100
DEG C, after rotating speed is stirred to react 30~50min under conditions of being 250~350r/min, mixed liquor is obtained, mixed liquor and formaldehyde are pressed into matter
Measure ratio 8：1~8：2 mixing, and the sulfurous of 0.1~0.3 times of mixed liquor quality is added in into the mixture of mixed liquor and formaldehyde successively
Sour sodium, the dimethylamine and the 1- bromobutane of 0.3~0.4 times of mixed liquor quality that 0.2~0.3 times of mixed liquor quality, in temperature be 65
~85 DEG C, after rotating speed is stirred 3~5h under conditions of being 230~330r/min, both sexes sulfonated phenol formaldehyde resin blank is obtained, by two
After property sulfonated phenol formaldehyde resin blank is washed with deionized 3~8 times, and by the both sexes sulfonated phenol formaldehyde resin blank and matter after washing
Measure the ethanol solution in mass ratio 1 that score is 30~40%：5~1：10 mixing, after 20~30h is impregnated under room temperature, mistake
Filter, obtains filter cake, and dry 20~30min under conditions of being 75~85 DEG C in temperature by filter cake obtains both sexes sulfonated phenol formaldehyde resin；It will be different
Fluorine that ketone diisocyanate and polypropylene glycol in mass ratio 1：1~2：1 mixing, and to isoflurane chalcone diisocyanate and poly- the third two
The dibutyl tin laurate of 0.1~0.2 times of isoflurane chalcone diisocyanate quality is added in the mixture of alcohol, obtains isophorone
Diisocyanate mixed liquor is passed through nitrogen into isoflurane chalcone diisocyanate mixed liquor with the rate of 20~40mL/min, and
It is 80~90 DEG C in temperature, under conditions of rotating speed is 250~300r/min, after being stirred 1~2h, obtains two isocyanide of isophorone
Acid esters reaction solution；By isoflurane chalcone diisocyanate reaction solution and dihydromethyl propionic acid in mass ratio 5：2~5：3 mixing, and to
Isoflurane chalcone diisocyanate reaction solution is added in the mixture of isoflurane chalcone diisocyanate reaction solution and dihydromethyl propionic acid
The 1,4-butanediol that 0.1~0.3 times of quality obtains isoflurane chalcone diisocyanate dihydromethyl propionic acid mixture, to isophorone
Nitrogen is passed through with the rate of 20~40mL/min in diisocyanate dihydromethyl propionic acid mixture, and in temperature be 80~90
DEG C, after rotating speed is stirred to react 80~120min under conditions of being 230~300r/min, blank liquid must be pre-processed, base will be pre-processed
Feed liquid is cooled to 70~75 DEG C, and by the pretreatment blank liquid after cooling and silane coupling agent in mass ratio 3：1~3：2 mixing,
And the acetone of 0.1~0.2 times of pretreatment blank liquid quality is added in into the mixture of pretreatment blank liquid and silane coupling agent, it obtains
The silane coupled agent composition of blank liquid is pre-processed, into the pretreatment silane coupled agent composition of blank liquid with 20~40mL/min's
Rate is passed through nitrogen, and is 65~75 DEG C in temperature, and rotating speed is stirred 80~100min under conditions of being 250~300r/min
Afterwards, obtain blank liquid, after blank liquid is cooled to 35~45 DEG C with triethylamine in mass ratio 5：1~5：2 mixing, in temperature for 30~
40 DEG C, under conditions of rotating speed is 300~320r/min, after being stirred 15~20min, blank liquid must be pre-processed, will be pre-processed
Blank liquid moves into Rotary Evaporators, and in 40~45 DEG C of temperature, rotating speed is 100~120r/min, and pressure is 0.04~0.08MPa's
Under the conditions of after 30~50min of spin concentration, obtain polyurethane dispersing liquid；Both sexes sulfonated phenol formaldehyde resin and polyurethane dispersing liquid are pressed into matter
Measure ratio 3：2~3：1 is mixed in blender, and changing for 0.2~0.3 times of both sexes sulfonated phenol formaldehyde resin quality is added in into blender
Property graphene oxide and 0.06~0.12 times of both sexes sulfonated phenol formaldehyde resin quality dispersant, in temperature be 45~65 DEG C, rotating speed
After being stirred 10~20min under conditions of 250~300r/min, heat resistant type fluid loss additive is obtained.The silane coupling agent is
Any one in silane resin acceptor kh-550, silane coupling agent KH-560 or Silane coupling reagent KH-570.The modified oxidized stone
The preparation method of black alkene is by graphene oxide sonic oscillation, and after centrifugation, concentrated by rotary evaporation is dry, must pre-process oxidation stone
Black alkene, by pretreatment graphene oxide and silane coupling agent KH-560 in mass ratio 1：3~1：5 mixing, and add in pretreatment oxygen
The water of 20~30 times of graphite alkene quality after being stirred, filters, dry, obtains modified graphene oxide.The dispersant is divides
Any one in powder MF, dispersant NNO or dispersant 5040.
Example 1
By phenol and formaldehyde in mass ratio 4：2 are mixed in beaker, with the sodium hydroxide solution that mass fraction is 8%
It adjusts in beaker after pH to 8, beaker is moved into digital display constant temperature blender with magnetic force, be 100 DEG C in temperature, rotating speed is 350r/min's
Under the conditions of be stirred to react 50min after, mixed liquor is obtained, by mixed liquor and formaldehyde in mass ratio 8：2 mixing, and successively to mixed liquor with
The sodium sulfite of 0.3 times of mixed liquor quality, the dimethylamine and mixed liquor matter that 0.3 times of mixed liquor quality are added in the mixture of formaldehyde
The 1- bromobutane of 0.4 times of amount is 85 DEG C in temperature, after rotating speed is stirred 5h under conditions of being 330r/min, obtains both sexes sulfonation
Phenolic resin blank, after both sexes sulfonated phenol formaldehyde resin blank is washed with deionized 8 times, and by the both sexes sulphonated phenol after washing
Urea formaldehyde blank and the ethanol solution in mass ratio 1 that mass fraction is 40%：10 mixing, after 30h is impregnated under room temperature, mistake
Filter, obtains filter cake, and dry 30min under conditions of being 85 DEG C in temperature by filter cake obtains both sexes sulfonated phenol formaldehyde resin；By isophorone two
Isocyanates and polypropylene glycol in mass ratio 2：1 mixing, and into the mixture of isoflurane chalcone diisocyanate and polypropylene glycol
The dibutyl tin laurate of 0.2 times of isoflurane chalcone diisocyanate quality is added in, obtains isoflurane chalcone diisocyanate mixed liquor,
Nitrogen is passed through with the rate of 40mL/min into isoflurane chalcone diisocyanate mixed liquor, and is 90 DEG C in temperature, rotating speed is
Under conditions of 300r/min, after being stirred 2h, isoflurane chalcone diisocyanate reaction solution is obtained；By isoflurane chalcone diisocyanate
Reaction solution and dihydromethyl propionic acid in mass ratio 5：3 mixing, and to isoflurane chalcone diisocyanate reaction solution and dihydroxymethyl third
The 1,4-butanediol of 0.3 times of isoflurane chalcone diisocyanate reaction solution quality is added in the mixture of acid, it is different to obtain isophorone two
Cyanate dihydromethyl propionic acid mixture, into isoflurane chalcone diisocyanate dihydromethyl propionic acid mixture with 40mL/min's
Rate is passed through nitrogen, and is 90 DEG C in temperature, after rotating speed is stirred to react 120min under conditions of being 300r/min, obtains pretreatment base
Pretreatment blank liquid is cooled to 75 DEG C by feed liquid, and by the pretreatment blank liquid after cooling and silane coupling agent in mass ratio 3：2
Mixing, and the acetone for pre-processing 0.2 times of blank liquid quality is added in into the mixture of pretreatment blank liquid and silane coupling agent, it obtains
The silane coupled agent composition of blank liquid is pre-processed, into the pretreatment silane coupled agent composition of blank liquid with the rate of 40mL/min
Nitrogen is passed through, and is 75 DEG C in temperature, after rotating speed is stirred 100min under conditions of being 300r/min, blank liquid is obtained, by base
Feed liquid be cooled to 45 DEG C after with triethylamine in mass ratio 5：2 mixing, in temperature be 40 DEG C, rotating speed be 320r/min under conditions of,
After being stirred 20min, blank liquid must be pre-processed, pretreatment blank liquid is moved into Rotary Evaporators, in temperature 45 C, rotating speed is
120r/min under conditions of pressure is 0.08MPa after spin concentration 50min, obtains polyurethane dispersing liquid；By both sexes sulfonated phenolic tree
Fat and polyurethane dispersing liquid in mass ratio 3：1 is mixed in blender, and both sexes sulfonated phenol formaldehyde resin matter is added in into blender
Amount 0.3 times modified graphene oxide and 0.12 times of both sexes sulfonated phenol formaldehyde resin quality dispersant, in temperature be 65 DEG C, rotating speed
After being stirred 20min under conditions of 300r/min, heat resistant type fluid loss additive is obtained.The silane coupling agent is silane coupling agent
KH-550.The preparation method of the modified graphene oxide is by graphene oxide sonic oscillation, and after centrifugation, revolving is dense
Contracting, it is dry, pretreatment graphene oxide is obtained, by pretreatment graphene oxide and silane coupling agent KH-560 in mass ratio 1：5 is mixed
It closes, and adds in the water of 30 times of pretreatment graphene oxide quality, after being stirred, filter, it is dry, obtain modified graphene oxide.
The dispersant is Dispersant MF.
Example 2
By phenol and formaldehyde in mass ratio 4：2 are mixed in beaker, with the sodium hydroxide solution that mass fraction is 8%
It adjusts in beaker after pH to 8, beaker is moved into digital display constant temperature blender with magnetic force, be 100 DEG C in temperature, rotating speed is 350r/min's
Under the conditions of be stirred to react 50min after, mixed liquor is obtained, by mixed liquor and formaldehyde in mass ratio 8：2 mixing, and successively to mixed liquor with
The sodium sulfite of 0.3 times of mixed liquor quality, the dimethylamine and mixed liquor matter that 0.3 times of mixed liquor quality are added in the mixture of formaldehyde
The 1- bromobutane of 0.4 times of amount is 85 DEG C in temperature, after rotating speed is stirred 5h under conditions of being 330r/min, obtains both sexes sulfonation
Phenolic resin blank, after both sexes sulfonated phenol formaldehyde resin blank is washed with deionized 8 times, and by the both sexes sulphonated phenol after washing
Urea formaldehyde blank and the ethanol solution in mass ratio 1 that mass fraction is 40%：10 mixing, after 30h is impregnated under room temperature, mistake
Filter, obtains filter cake, and dry 30min under conditions of being 85 DEG C in temperature by filter cake obtains both sexes sulfonated phenol formaldehyde resin；By both sexes sulphonated phenol
Urea formaldehyde and modified graphene oxide in mass ratio 10：3 are mixed in blender, and both sexes sulfonated phenolic is added in into blender
The dispersant that 0.12 times of resin quality is 65 DEG C in temperature, after rotating speed is stirred 20min under conditions of being 300r/min, obtains
Heat resistant type fluid loss additive.The preparation method of the modified graphene oxide be by graphene oxide sonic oscillation, after centrifugation,
Concentrated by rotary evaporation, it is dry, pretreatment graphene oxide is obtained, by pretreatment graphene oxide with silane coupling agent KH-560 in mass ratio
1：5 mixing, and the water of 30 times of pretreatment graphene oxide quality is added in, after being stirred, filter, it is dry, obtain modified oxidized stone
Black alkene.The dispersant is Dispersant MF.
Example 3
By phenol and formaldehyde in mass ratio 4：2 are mixed in beaker, with the sodium hydroxide solution that mass fraction is 8%
It adjusts in beaker after pH to 8, beaker is moved into digital display constant temperature blender with magnetic force, be 100 DEG C in temperature, rotating speed is 350r/min's
Under the conditions of be stirred to react 50min after, mixed liquor is obtained, by mixed liquor and formaldehyde in mass ratio 8：2 mixing, and successively to mixed liquor with
The sodium sulfite of 0.3 times of mixed liquor quality, the dimethylamine and mixed liquor matter that 0.3 times of mixed liquor quality are added in the mixture of formaldehyde
The 1- bromobutane of 0.4 times of amount is 85 DEG C in temperature, after rotating speed is stirred 5h under conditions of being 330r/min, obtains both sexes sulfonation
Phenolic resin blank, after both sexes sulfonated phenol formaldehyde resin blank is washed with deionized 8 times, and by the both sexes sulphonated phenol after washing
Urea formaldehyde blank and the ethanol solution in mass ratio 1 that mass fraction is 40%：10 mixing, after 30h is impregnated under room temperature, mistake
Filter, obtains filter cake, and dry 30min under conditions of being 85 DEG C in temperature by filter cake obtains both sexes sulfonated phenol formaldehyde resin；By isophorone two
Isocyanates and polypropylene glycol in mass ratio 2：1 mixing, and into the mixture of isoflurane chalcone diisocyanate and polypropylene glycol
The dibutyl tin laurate of 0.2 times of isoflurane chalcone diisocyanate quality is added in, obtains isoflurane chalcone diisocyanate mixed liquor,
Nitrogen is passed through with the rate of 40mL/min into isoflurane chalcone diisocyanate mixed liquor, and is 90 DEG C in temperature, rotating speed is
Under conditions of 300r/min, after being stirred 2h, isoflurane chalcone diisocyanate reaction solution is obtained；By isoflurane chalcone diisocyanate
Reaction solution and dihydromethyl propionic acid in mass ratio 5：3 mixing, and to isoflurane chalcone diisocyanate reaction solution and dihydroxymethyl third
The 1,4-butanediol of 0.3 times of isoflurane chalcone diisocyanate reaction solution quality is added in the mixture of acid, it is different to obtain isophorone two
Cyanate dihydromethyl propionic acid mixture, into isoflurane chalcone diisocyanate dihydromethyl propionic acid mixture with 40mL/min's
Rate is passed through nitrogen, and is 90 DEG C in temperature, after rotating speed is stirred to react 120min under conditions of being 300r/min, obtains pretreatment base
Pretreatment blank liquid is cooled to 75 DEG C by feed liquid, and by the pretreatment blank liquid after cooling and silane coupling agent in mass ratio 3：2
Mixing, and the acetone for pre-processing 0.2 times of blank liquid quality is added in into the mixture of pretreatment blank liquid and silane coupling agent, it obtains
The silane coupled agent composition of blank liquid is pre-processed, into the pretreatment silane coupled agent composition of blank liquid with the rate of 40mL/min
Nitrogen is passed through, and is 75 DEG C in temperature, after rotating speed is stirred 100min under conditions of being 300r/min, blank liquid is obtained, by base
Feed liquid be cooled to 45 DEG C after with triethylamine in mass ratio 5：2 mixing, in temperature be 40 DEG C, rotating speed be 320r/min under conditions of,
After being stirred 20min, blank liquid must be pre-processed, pretreatment blank liquid is moved into Rotary Evaporators, in temperature 45 C, rotating speed is
120r/min under conditions of pressure is 0.08MPa after spin concentration 50min, obtains polyurethane dispersing liquid；By both sexes sulfonated phenolic tree
Fat and polyurethane dispersing liquid in mass ratio 3：1 is mixed in blender, and both sexes sulfonated phenol formaldehyde resin matter is added in into blender
The dispersant of 0.12 times of amount is 65 DEG C in temperature, after rotating speed is stirred 20min under conditions of being 300r/min, obtains heat resistant type
Fluid loss additive.The silane coupling agent is silane resin acceptor kh-550.The dispersant is Dispersant MF.
Comparative example：
The heat resistant type fluid loss additive of 1 to 3 gained of example and comparative example product are subjected to performance detection, specific detection method is as follows：
Filtration reduction and heat resistance：20g sodium bentonites and 1g sodium carbonate, high-speed stirred are added in 200mL deionized waters
20min places maintenance and is starched for 24 hours to get 10% base at room temperature；1% fluid loss additive, the press filtration in are added in the base slurry prepared
Commit a breach of etiquette and survey the middle filter pressing loss of drilling fluid, with the high filter pressing loss of high pressure high temperature filter tester pyrometry, add in prescribed volume solution in
Aging roller, filter pressing loss, high temperature and high pressure filter loss in being surveyed after 140 DEG C of rolling aging 16h（180℃、3.5MPa）.
Specific testing result is as shown in table 1：
Table 1：Filtration reduction and the specific testing result of heat resistance
By 1 testing result of table it is found that heat resistant type fluid loss additive prepared by technical solution of the present invention have excellent filtration reduction and
The characteristics of heat resistance, has broad prospects in the development of fluid loss additive industry.
Claims (4)
1. a kind of preparation method of heat resistant type fluid loss additive, it is characterised in that specifically preparation process is：
（1）By phenol and formaldehyde in mass ratio 3：2~4：2 mixing, after adjusting pH, are stirred to react, obtain mixed liquor, will
Mixed liquor and formaldehyde in mass ratio 8：1~8：2 mixing, and the sodium sulfite of 0.1~0.3 times of mixed liquor quality is sequentially added, it mixes
The dimethylamine of 0.2~0.3 times of liquid quality and the 1- bromobutane of 0.3~0.4 times of mixed liquor quality are closed, after being stirred, obtains both sexes
Sulfonated phenol formaldehyde resin blank washs both sexes sulfonated phenol formaldehyde resin blank 3~8 times, and by the both sexes sulfonated phenolic tree after washing
Fat blank and ethanol solution in mass ratio 1：5~1：10 mixing are impregnated, and are filtered, dry, obtain both sexes sulfonated phenol formaldehyde resin；
（2）By isoflurane chalcone diisocyanate and polypropylene glycol in mass ratio 1：1~2：1 mixing, and it is different to add in isophorone two
The dibutyl tin laurate that 0.1~0.2 times of cyanate quality obtains isoflurane chalcone diisocyanate mixed liquor, by isophorone
Diisocyanate mixed liquor heating stirring under nitrogen atmosphere is reacted, and obtains isoflurane chalcone diisocyanate reaction solution；
（3）By isoflurane chalcone diisocyanate reaction solution and dihydromethyl propionic acid in mass ratio 5：2~5：3 mixing, and add in different
The 1,4-butanediol of your 0.1~0.3 times of ketone di-isocyanate reaction liquid quality of fluorine, is stirred to react under nitrogen guard mode, obtains
Blank liquid is pre-processed, by pretreatment blank liquid cooling, and by the pretreatment blank liquid after cooling and silane coupling agent in mass ratio
3：1~3：2 mixing add in the acetone of 0.1~0.2 times of pretreatment blank liquid quality, are stirred under nitrogen atmosphere, obtain blank
Liquid, by blank liquid cool down after with triethylamine in mass ratio 5：1~5：2 mixing, spin concentration obtain polyurethane dispersing liquid；
（4）By both sexes sulfonated phenol formaldehyde resin and polyurethane dispersing liquid in mass ratio 3：2~3：1 mixing, and add in both sexes sulphonated phenol
The modified graphene oxide and the dispersion of 0.06~0.12 times of both sexes sulfonated phenol formaldehyde resin quality that 0.2~0.3 times of urea formaldehyde quality
Agent after being stirred, obtains heat resistant type fluid loss additive.
2. a kind of preparation method of heat resistant type fluid loss additive according to claim 1, it is characterised in that：Step（3）It is described
Silane coupling agent is silane resin acceptor kh-550, any one in silane coupling agent KH-560 or Silane coupling reagent KH-570.
3. a kind of preparation method of heat resistant type fluid loss additive according to claim 1, it is characterised in that：Step（4）It is described
The preparation method of modified graphene oxide is by graphene oxide sonic oscillation, and after centrifugation, concentrated by rotary evaporation is dry, obtains pre-
Graphene oxide is handled, by pretreatment graphene oxide and silane coupling agent KH-560 in mass ratio 1：3~1：5 mixing, and add
Enter to pre-process the water of 20~30 times of graphene oxide quality, after being stirred, filter, it is dry, obtain modified graphene oxide.
4. a kind of preparation method of heat resistant type fluid loss additive according to claim 1, it is characterised in that：Step（4）It is described
Dispersant is Dispersant MF, any one in dispersant NNO or dispersant 5040.
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