CN108250376A - Water-soluble Cementing preparation method of phenolic resin and its device - Google Patents
Water-soluble Cementing preparation method of phenolic resin and its device Download PDFInfo
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- CN108250376A CN108250376A CN201711366641.9A CN201711366641A CN108250376A CN 108250376 A CN108250376 A CN 108250376A CN 201711366641 A CN201711366641 A CN 201711366641A CN 108250376 A CN108250376 A CN 108250376A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
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Abstract
The present invention discloses a kind of water-soluble Cementing preparation method of phenolic resin and its device, belong to the phenolic resins field in same with thermosetting compound material, including valve, filter device, bobbing machine, cleaning device, steel pipe and raw material cabin, raw material cabin is sequentially connected bobbing machine by steel pipe, cleaning device, filter device and valve, valve is fixed on the end of steel pipe, the filter device is by coarse granule filter layer, fine grained filter layer and core filter layer composition, coarse granule filter layer wraps up fine grained filter layer, fine grained filter layer wraps up core filter layer, the cleaning device surface is iron sheet successively from inside to outside, PVC plastic and high density numerical value composition;More preferably, cost is lower for thickening effect, and using more convenient, solidification effect is significantly improved with efficiency, the oil-well cement solidification intensity higher of well cementation.
Description
Technical field
The present invention relates to a kind of water-soluble Cementing preparation method of phenolic resin and its devices, belong to thermosetting property and answer
Phenolic resins field in condensation material.
Background technology
Phenolic resin is in recent years, to be actively researched and developed water both at home and abroad using one of earliest synthetic material in the world
Dissolubility phenolic resin, because it is simple with production procedure, raw material resources are abundant, price is relatively low and the resin is had in itself
Standby fusibility, molding bonded are good, the good characteristics of heat resistance height, completion of cure etc., be widely used in electric insulation,
The industry-by-industries such as pressing plate adhesive, anti-corrosion of metal antirust and aqueous-based polymers gel cross-linkage agent, in particular for being bored with oil gas field
The depth profile control agent that spy mud and the well cementation additional thickener of oil-well cement mortar and mid-late oilfield development are applied this
A little exploitation of oil-gas field industries, with the rapid development of global economy, oil is as high efficient energy sources, finiteness and war because of its resource
Slightly importance, is increasingly becoming a kind of indispensable strategic materials, is directly related to a national energy security and economic hair
Exhibition.Chinese society economy maintains sustained and rapid growth, and petroleum reserves and yield are difficult to meet the needs that consumption increases, and imbalance between supply and demand is year by year
It increases and becomes increasingly conspicuous, the external dependence degree of China's oil is estimated at present has reached 60% or so.In order to alleviate this contradiction, remove
It taps a new source of energy, strengthen except the exploration to new oil field, the main means taken are exactly the recovery ratio for improving oil field, including
The raising of oil well cementing technology etc. reduces waste of the oil in recovery process.
Invention content
In view of the above existing problems in the prior art, the present invention provides a kind of water-soluble Cementing phenolic resin-mades
Preparation Method and its device, the sedimentation stability of mixture, pumpability and filling process is more preferable, alternative traditional by having
The thickener or non-ionic polyurethane class thickener of the acrylate polymer of synergistic effect and bentonite mixtures composition, and
More preferably, cost is lower for thickening effect, and using more convenient, solidification effect is significantly improved with efficiency, and the oil-well cement curing of well cementation is by force
Spend higher.
To achieve these goals, a kind of water-soluble Cementing preparation method of phenolic resin for using of the present invention and
Its device, including valve, filter device, bobbing machine, cleaning device, steel pipe and raw material cabin, raw material cabin is sequentially connected by steel pipe
Bobbing machine, cleaning device, filter device and valve, valve are fixed on the end of steel pipe, and the filter device is by coarse granule
Filter layer, fine grained filter layer and core filter layer composition, coarse granule filter layer package fine grained filter layer, fine grained filter layer
Core filter layer is wrapped up, the cleaning device surface is iron sheet, PVC plastic and high density numerical value composition successively from inside to outside.
The coarse granule filter layer of the filter device is 15 mesh, and fine grained filter layer is 25 mesh, and core filter layer is 50
Mesh.
The raw material cabin surface is covered with cover board.
The phenol, formaldehyde, catalyst proportioning be:
Phenol:1 part;
Formaldehyde (44%):Mole ratio with phenol is 1:0.85~1.3;
Catalyst:Calcium hydroxide accounts for the 0.5~0.8% of phenol and formaldehyde otal investment.
A kind of preparation of water-soluble Cementing phenolic resin material, preparation process are as follows:
A, it feeds intake:The phenol, catalyst or formaldehyde that are weighed by quantitative number are put into reaction kettle, starting blender makes benzene
Phenol, catalyst or formaldehyde are mixed evenly, and are opened steam valve and are begun to warm up;
B, dropwise reaction:When reactor temperature is warming up to 80-90 DEG C, start that quantitative catalyst or formaldehyde is added dropwise,
Time for adding is 1-3.5 hours or so;If temperature in the kettle is warming up to 100-105 DEG C, answers steam off, continue to stir;
C, polycondensation reaction:After being added dropwise, material in kettle should be observed at any time, when finding that material starts emulsification, opened again
It opens preventing trace amount of steam to be kept the temperature, the reaction was continued at a temperature of 100-120 DEG C 2-4 hours;
D, after insulation reaction, increase steam is heated, temperature in the kettle heating, until stop stirring at 140-150 DEG C,
Steam off valve adjusts pipeline valve, starts the dehydration of nature normal pressure, should observe the flowmeter of wastewater storage tank at this time, and dehydrating amount is
The 8-10% of input material total amount;
E, it after reaching dehydration terminal, is then turned on stirring, opens cooling water valve, carry out chuck cooling, treat material temperature in kettle
After degree is less than 60 DEG C, stirring, cooling water valve are closed, carries out blowing, finally obtains the naval stores of light brown liquid state.
The phenol is the industrial synthesizing phenol that cumene method or sulfonation method are produced, and the formaldehyde is by methanol oxygen
Its content of industrial formaldehyde solution made from change method is 44%, and the catalyst is the hydroxide in alkaline earth metal hydroxide
Calcium.
This water-soluble Cementing phenolic resin has the following advantages that compared with organic solvent type phenolic resin:1. into
This is low;It is 2. free from environmental pollution;It is 3. nontoxic;It is 4. nonflammable explosive;It is 5. safe;6. with existing oil-well cement system phase
Capacitive, mixture are preferable.Therefore, the theoretical research and popularization and application of water soluble phenol resin meets current economic, environmental protection, height
The demand for development of effect has broad application prospects and good social value, and the water solubility of phenolic resin depends on benzene
The dissolubility of the reaction product of phenol and formaldehyde in aqueous solution, if product molecule polarity is big, then its dissolubility in water
Greatly, resin is less prone to emulsification lamination.Selection is matched using suitable, the appropriate reaction temperature of different phenol formaldehyde ratios, control
Degree and conversion process parameter, process conditions regulate and control reaction speed;Suitable alkali and alkaline earth metal ions hydroxide is selected to make
For catalyst, phenol and formaldehyde is promoted to carry out methylolation addition reaction, explore the speed of addition reaction than condensation reaction speed
It is mainly the phenolic alcohol rich in methylol to spend the product to be fast, generated in this way, and wherein methylol is the stronger active group of polarity,
Its content is more, and the polarity of resin is stronger, water-soluble better;The appropriate dosage for increasing formaldehyde, also contributes to hydroxymethyl phenol
Generation improves the water solubility of phenolic resin.
Description of the drawings
Fig. 1 is the structural diagram of the present invention;
In figure:1st, valve, 2, filter device, 3, bobbing machine, 4, cleaning device, 5, steel pipe, 6, raw material cabin.
Specific embodiment
Understand to make the object, technical solutions and advantages of the present invention clearer, it is right below by attached drawing and embodiment
The present invention is further elaborated.However, it should be understood that specific embodiment described herein is only used to explain this hair
Range that is bright, being not intended to restrict the invention.
As shown in Figure 1, this water-soluble Cementing preparation method of phenolic resin and its device, including valve 1, filtering
Device 2, bobbing machine 3, cleaning device 4, steel pipe 5 and raw material cabin 6, raw material cabin 6 is sequentially connected bobbing machine 3 by steel pipe 5, cleaning fills
Put 4, filter device 2 and valve 1, valve 1 is fixed on the end of steel pipe 5, the filter device 2 be by coarse granule filter layer,
Fine grained filter layer and core filter layer composition, coarse granule filter layer package fine grained filter layer, fine grained filter layer package core
Heart filter layer, 4 surface of cleaning device are iron sheet, PVC plastic and high density numerical value composition successively from inside to outside.
The coarse granule filter layer of the filter device 2 is 15 mesh, and fine grained filter layer is 25 mesh, and core filter layer is 50
Mesh, pilot production find that, when coarse granule filter layer is 15 mesh, fine grained filter layer is 25 mesh, and core filter layer is 50 in the process
During mesh, the effect for filtering phenolic resin is good, does not have trash flow and enters next stage.
6 surface of raw material cabin can effectively prevent impurity and enter inside raw material cabin 6 covered with cover board.
The phenol, formaldehyde, catalyst proportioning be:
Phenol:1 part;
Formaldehyde (44%):Mole ratio with phenol is 1:0.85~1.3;
Catalyst:Calcium hydroxide accounts for the 0.5~0.8% of phenol and formaldehyde otal investment.
A kind of preparation of water-soluble Cementing phenolic resin material, preparation process are as follows:
A, it feeds intake:The phenol, catalyst or formaldehyde that are weighed by quantitative number are put into reaction kettle, starting blender makes benzene
Phenol, catalyst or formaldehyde are mixed evenly, and are opened steam valve and are begun to warm up;
B, dropwise reaction:When reactor temperature is warming up to 80-90 DEG C, start that quantitative catalyst or formaldehyde is added dropwise,
Time for adding is 1-3.5 hours or so;If temperature in the kettle is warming up to 100-105 DEG C, answers steam off, continue to stir;
C, polycondensation reaction:After being added dropwise, material in kettle should be observed at any time, when finding that material starts emulsification, opened again
It opens preventing trace amount of steam to be kept the temperature, the reaction was continued at a temperature of 100-120 DEG C 2-4 hours;
D, after insulation reaction, increase steam is heated, temperature in the kettle heating, until stop stirring at 140-150 DEG C,
Steam off valve adjusts pipeline valve, starts the dehydration of nature normal pressure, should observe the flowmeter of wastewater storage tank at this time, and dehydrating amount is
The 8-10% of input material total amount;
E, it after reaching dehydration terminal, is then turned on stirring, opens cooling water valve, carry out chuck cooling, treat material temperature in kettle
After degree is less than 60 DEG C, stirring, cooling water valve are closed, carries out blowing, finally obtains the naval stores of light brown liquid state.
The phenol is the industrial synthesizing phenol that cumene method or sulfonation method are produced, and the formaldehyde is by methanol oxygen
Its content of industrial formaldehyde solution made from change method is 44%, and the catalyst is the hydroxide in alkaline earth metal hydroxide
Calcium.
Case is embodied
Below in conjunction with the embodiment of the present invention, the technical solution in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only the part of the embodiment of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, those of ordinary skill in the art's all other embodiments obtained without making creative work,
It shall fall within the protection scope of the present invention.
Embodiment 1
In the embodiment of the present invention, a kind of water soluble phenol resin, raw material includes phenol, paraformaldehyde and catalyst,
The mole ratio of middle phenol and formaldehyde is 1:0.85, catalyst (sodium hydroxide) account for phenol, formaldehyde otal investment 0.8%.
A kind of water-soluble Cementing preparation method of phenolic resin, is as follows:
(1) phenol and formaldehyde are added to and condenser, thermometer (band thermocouple), blender and constant pressure addition leakage is installed
In the reaction kettle device of bucket, starting blender is mixed evenly phenol, formaldehyde, opens steam valve and begins to warm up;
(2) when reactor temperature being warming up to 80 DEG C, the calcium hydroxide of quantitative half is added;Steam off, continuation
Stirring when temperature in the kettle warms naturally to 85 DEG C, starts that (having dissolved in advance) remaining calcium hydroxide, time for adding is added dropwise
It is 1 hour or so;
(3) after being added dropwise, material in kettle should be observed at any time, when finding that material starts emulsification, be again turned on micro steaming
Vapour is kept the temperature, and the reaction was continued at a temperature of 100-110 DEG C 2 hours;
(4) after insulation reaction, increase steam be heated to stopping stirring, steam off valve, regulation pipe at 140 DEG C
Road valve starts the dehydration of nature normal pressure, should observe the flowmeter of wastewater storage tank at this time, and dehydrating amount is input material total amount
10%;(5) it after reaching dehydration terminal, is then turned on stirring, opens cooling water valve, carry out chuck cooling, treat material temperature in kettle
After 60 DEG C, stirring, cooling water valve are closed, carries out blowing, finally obtains the naval stores of light brown liquid state.
Calcium hydroxide is simultaneously as the catalyst reacted between phenol and formaldehyde.
Case study on implementation 2:
In the embodiment of the present invention, a kind of water soluble phenol resin, raw material includes phenol, paraformaldehyde and catalyst,
The mole ratio of middle phenol and formaldehyde is 1:1, catalyst (sodium hydroxide) account for phenol, formaldehyde otal investment 0.7%.
A kind of water-soluble Cementing preparation method of phenolic resin, is as follows:
(1) phenol and formaldehyde are added to and condenser, thermometer (band thermocouple), blender and constant pressure addition leakage is installed
In the reaction kettle device of bucket, starting blender is mixed evenly phenol, formaldehyde, opens steam valve and begins to warm up;
(2) when reactor temperature being warming up to 80 DEG C or more, start that (having dissolved in advance) quantitative hydroxide is added dropwise
Calcium adds in constant pressure funnel, and time for adding is 2 hours or so;If temperature in the kettle is warming up to 105 DEG C or more, steaming should be closed
Vapour continues to stir;
(3) after being added dropwise, material in kettle should be observed at any time, when finding that material starts emulsification, be again turned on micro steaming
Vapour is kept the temperature, and the reaction was continued at a temperature of 100-110 DEG C 2-3 hours;
(4) after insulation reaction, increase steam is heated, and temperature in the kettle heating until stopping stirring at 140 DEG C, is closed
Steam valve is closed, adjusts pipeline valve, starts the dehydration of nature normal pressure, the flowmeter of wastewater storage tank should be observed at this time, dehydrating amount is institute
Put into the 10% of material total amount;
(5) it after reaching dehydration terminal, is then turned on stirring, opens cooling water valve, carry out chuck cooling, treat material temperature in kettle
After degree is less than 60 DEG C, stirring, cooling water valve are closed, carries out blowing, finally obtains the naval stores of light brown liquid state.
Calcium hydroxide is simultaneously as the catalyst reacted between phenol and formaldehyde.
Case study on implementation 3:
In the embodiment of the present invention, a kind of water soluble phenol resin, raw material includes phenol, paraformaldehyde and catalyst,
The mole ratio of middle phenol and formaldehyde is 1:1.1, catalyst (sodium hydroxide) account for phenol, formaldehyde otal investment 0.6%.
A kind of water-soluble Cementing preparation method of phenolic resin, is as follows:
(1) formaldehyde of phenol, calcium hydroxide and quantitative half is added to and condenser, thermometer (band thermoelectricity is installed
Occasionally), in the reaction kettle device of blender and constant pressure funnel, starting blender makes phenol, formaldehyde, calcium hydroxide mix
It is even, it opens steam valve and begins to warm up;
(2) when reactor temperature being warming up to 90 DEG C or more, start to be added dropwise the formaldehyde of quantitative remaining half, during dropwise addition
Between be 2.5 hours or so;If temperature in the kettle is warming up to 105 DEG C or more, answers steam off, continue to stir;
(3) after being added dropwise, material in kettle should be observed at any time, when finding that material starts emulsification, be again turned on micro steaming
Vapour is kept the temperature, and the reaction was continued at a temperature of 110-120 DEG C 2-3 hours;
(4) after insulation reaction, increase steam is heated, and temperature in the kettle heating until stopping stirring at 140 DEG C, is closed
Steam valve is closed, adjusts pipeline valve, starts the dehydration of nature normal pressure, the flowmeter of wastewater storage tank should be observed at this time, dehydrating amount is institute
Put into the 10% of material total amount;
(5) it after reaching dehydration terminal, is then turned on stirring, opens cooling water valve, carry out chuck cooling, treat material temperature in kettle
After degree is less than 60 DEG C, stirring, cooling water valve are closed, carries out blowing, finally obtains the naval stores of light brown liquid state.
Calcium hydroxide is simultaneously as the catalyst reacted between phenol and formaldehyde.
Case study on implementation 4:
In the embodiment of the present invention, a kind of water soluble phenol resin, raw material includes phenol, paraformaldehyde and catalyst,
The mole ratio of middle phenol and formaldehyde is 1:1.2, catalyst (sodium hydroxide) account for phenol, formaldehyde otal investment 0.5%.
A kind of water-soluble Cementing preparation method of phenolic resin, is as follows:
(1) phenol and calcium hydroxide are added to and condenser, thermometer (band thermocouple), blender and constant pressure drop is installed
In the reaction kettle device of liquid funnel, starting blender is mixed evenly phenol, calcium hydroxide, opens steam valve and begins to warm up;
(2) when reactor temperature being warming up to 85 DEG C or more, start that quantitative formaldehyde, time for adding 3-3.5 is added dropwise
Hour or so;If temperature in the kettle is warming up to 100 DEG C or more, answers steam off, continue to stir;
(3) after being added dropwise, material in kettle should be observed at any time, when finding that material starts emulsification, be again turned on micro steaming
Vapour is kept the temperature, and the reaction was continued under 105-110 DEG C of temperature condition 3 hours;
(4) after insulation reaction, increase steam is heated, and temperature in the kettle heating until stopping stirring at 145 DEG C, is closed
Steam valve is closed, adjusts pipeline valve, starts the dehydration of nature normal pressure, the flowmeter of wastewater storage tank should be observed at this time, dehydrating amount is institute
Put into the 8% of material total amount;
(5) it after reaching dehydration terminal, is then turned on stirring, opens cooling water valve, carry out chuck cooling, treat material temperature in kettle
After degree is less than 60 DEG C, stirring, cooling water valve are closed, carries out blowing, finally obtains the naval stores of light brown liquid state.
Calcium hydroxide is simultaneously as the catalyst reacted between phenol and formaldehyde.
Case study on implementation 5:
In the embodiment of the present invention, a kind of water soluble phenol resin, raw material includes phenol, paraformaldehyde and catalyst,
The mole ratio of middle phenol and formaldehyde is 1:1.3, catalyst (sodium hydroxide) account for phenol, formaldehyde otal investment 0.55%.
A kind of water-soluble Cementing preparation method of phenolic resin, is as follows:
(1) phenol and calcium hydroxide are added to and condenser, thermometer (band thermocouple), blender and constant pressure drop is installed
In the reaction kettle device of liquid funnel, starting blender is mixed evenly phenol, calcium hydroxide, opens steam valve and begins to warm up;
(2) when reactor temperature being warming up to 80 DEG C or more, start that quantitative formaldehyde is added dropwise, time for adding is small for 2.5
When or so;If temperature in the kettle is warming up to 100 DEG C or more, answers steam off, continue to stir;
(3) after being added dropwise, material in kettle should be observed at any time, when finding that material starts emulsification, be again turned on micro steaming
Vapour is kept the temperature, and the reaction was continued at a temperature of 110-120 DEG C 3-4 hours;
(4) after insulation reaction, increase steam is heated, and temperature in the kettle heating until stopping stirring at 150 DEG C, is closed
Steam valve is closed, adjusts pipeline valve, starts the dehydration of nature normal pressure, the flowmeter of wastewater storage tank should be observed at this time, dehydrating amount is institute
Put into the 9% of material total amount;
(5) it after reaching dehydration terminal, is then turned on stirring, opens cooling water valve, carry out chuck cooling, treat material temperature in kettle
After degree is less than 60 DEG C, stirring, cooling water valve are closed, carries out blowing, finally obtains the naval stores of light brown liquid state.
Calcium hydroxide is simultaneously as the catalyst reacted between phenol and formaldehyde.
By the water-soluble Cementing phenolic resin product that the embodiment above 1-5 and preparation method are obtained through surveying
Examination obtains technical indicator listed in Table:
Naval stores prepared by the present invention is after tested:Appearance:Thick liquid, the active ingredient of light brown:40% aqueous solution,
Viscosity:15,000-25,000cp、pH:7.0-8.0, free phenol:5.5-6.5%, melt water are than 1:7-8, molecular weight 3500-
6000.Batch test is carried out through research, in terms of mud fluid and the oil-well cement mortar well cementation thickener added outside all
Accreditation, the thickening that alternative traditional acrylate polymer by with synergistic effect is formed with bentonite mixtures are arrived
Agent or non-ionic polyurethane class thickener, the sedimentation stability of mixture, pumpability and filling process is more preferable, and cost
Lower, using more convenient, solidification effect is significantly improved with efficiency, the oil-well cement solidification intensity higher after well cementation.
The water soluble phenol resin of the present invention is by phenol, the mole ratio that formaldehyde is main Material synthesis, phenol and formaldehyde
It is 1:0.85~1.3, resin is in alkali and alkaline earth metal ions hydroxide ----calcium hydroxide as catalyst (account for about phenol,
The 0.5~0.8% of formaldehyde otal investment) promote matchmaker under conditions of by phenol with formaldehyde condensation into polymer, water is then prepared
Insoluble petroleum well cementation phenolic resin product.Due to product improve curing after water resistance, thickening while, cement bonded sand
The flow leveling of slurry is greatly improved, and has good thickening leveling effect, it can provide outstanding approximate Newtonian fluid
Flow leveling, excellent high thixotropic and preferable viscosity characteristics, and, phase helpful to the cement mortar solidification after thickening
Than the thickener that traditional acrylate polymer by with synergistic effect and bentonite mixtures form, xanthans class or non-
Ion polyurethanes thickener, for thickening effect it is stronger, can play alternative fiber element or swelling great soil group thickener spy
Special effect fruit can also be used cooperatively with traditional thickener;And since the resin is to belong to alkalescent product, even if temperature, pressure
Power changes, and the stability of viscosity is also quite outstanding, is particularly suitable in saline alkali geological environment (high-calcium ionic and high pH value).
The problem of oil-well cement mortar formula design (proportioning) is caused to be varied from thus, there is no the variation with winter, summer.
In addition, different with cellulose derivative, polyurethanes etc. be, it does not need to dissolve in advance, can be directly added into oil well water
In mud system, it can also be added in the mixing stage of cement mortar, therefore will be more widely used.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modification, equivalent replacement or improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of water-soluble Cementing preparation method of phenolic resin and its device, including valve (1), filter device (2),
Bobbing machine (3), cleaning device (4), steel pipe (5) and raw material cabin (6), which is characterized in that raw material cabin (6) by steel pipe (5) successively
Connection bobbing machine (3), cleaning device (4), filter device (2) and valve (1), valve (1) are fixed on the end of steel pipe (5), institute
The filter device (2) stated is made of coarse granule filter layer, fine grained filter layer and core filter layer, coarse granule filter layer package
Fine grained filter layer, fine grained filter layer package core filter layer, the cleaning device (4) surface is iron successively from inside to outside
Skin, PVC plastic and high density numerical value composition.
2. a kind of water-soluble Cementing preparation method of phenolic resin according to claim 1 and its device, special
Sign is that the coarse granule filter layer of the filter device (2) is 15 mesh, and fine grained filter layer is 25 mesh, and core filter layer is
50 mesh.
3. a kind of water-soluble Cementing preparation method of phenolic resin according to claim 1 and its device, special
Sign is that the raw material cabin (6) surface is covered with cover board.
A kind of 4. water-soluble Cementing preparation method of phenolic resin according to claim 1, which is characterized in that institute
The phenol stated, formaldehyde, catalyst proportioning be:
Phenol:1 part;
Formaldehyde (44%):Mole ratio with phenol is 1:0.85~1.3;
Catalyst:Calcium hydroxide accounts for the 0.5~0.8% of phenol and formaldehyde otal investment.
5. a kind of preparation of water-soluble Cementing phenolic resin material according to claim 4, preparation process is such as
Under:
A, it feeds intake:The phenol, catalyst or formaldehyde that are weighed by quantitative number are put into reaction kettle, starting blender makes phenol, urges
Agent or formaldehyde are mixed evenly, and are opened steam valve and are begun to warm up;
B, dropwise reaction:When reactor temperature is warming up to 80-90 DEG C, start that quantitative catalyst or formaldehyde is added dropwise, be added dropwise
Time is 1-3.5 hours or so;If temperature in the kettle is warming up to 100-105 DEG C, answers steam off, continue to stir;
C, polycondensation reaction:After being added dropwise, material in kettle should be observed at any time, when finding that material starts emulsification, be again turned on micro-
Amount steam is kept the temperature, and the reaction was continued at a temperature of 100-120 DEG C 2-4 hours;
D, after insulation reaction, increase steam is heated, and temperature in the kettle heating until stopping stirring at 140-150 DEG C, is closed
Steam valve adjusts pipeline valve, starts the dehydration of nature normal pressure, should observe the flowmeter of wastewater storage tank at this time, dehydrating amount is is thrown
Enter the 8-10% of material total amount;
E, it after reaching dehydration terminal, is then turned on stirring, opens cooling water valve, carry out chuck cooling, treat that material temperature in kettle is low
After 60 DEG C, stirring, cooling water valve are closed, carries out blowing, finally obtains the naval stores of light brown liquid state.
6. a kind of preparation of water-soluble Cementing phenolic resin material according to claim 4, which is characterized in that
The phenol is the industrial synthesizing phenol that cumene method or sulfonation method are produced, and the formaldehyde is is made by methanol oxidizing process
Industrial formaldehyde solution its content be 44%, the catalyst is the calcium hydroxide in alkaline earth metal hydroxide.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110760044A (en) * | 2019-11-11 | 2020-02-07 | 常熟东南塑料有限公司 | Phenolic resin for oil-gas field drilling thickener and preparation method thereof |
CN112094630A (en) * | 2020-11-17 | 2020-12-18 | 东营东方化学工业有限公司 | Composite component resin cross-linking agent and preparation method thereof |
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