CN102408882A - Phenol-urea-formaldhyde resin modified lignite filtrate loss reducer with high temperature resistance and salt tolerance, and its preparation method - Google Patents
Phenol-urea-formaldhyde resin modified lignite filtrate loss reducer with high temperature resistance and salt tolerance, and its preparation method Download PDFInfo
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Abstract
The invention relates to a preparation method of a filtrate loss reducer used for drilling fluids. With lignite as the main material, the method first prepares a sulfonated phenol-urea-formaldhyde resin mixture, which is then reacted with an alkaline solution and lignite, thus obtaining a sulfonated phenol-urea-formaldhyde resin modified lignite filtrate loss reducer. The lignite filtrate loss reducer comprises the following reactants by weight: 10%-20% of lignite; 2%-4% of one of or a mixture of NaOH and KOH; 50%-60% of water; 2%-5.5% of phenol; 8%-15% of formaldehyde; 3%-7% of urea; 0.15%-2% of a hydrolyzed acrylonitrile sodium salt; 0.125%-0.5% of polyacrylamide; and 2%-7% of a sulfonating agent (one of or a mixture of sodium sulfite, sodium bisulfite, and sodium metabisulfite).
Description
Technical field
The present invention relates to a kind of fluid loss additive for boring fluid and preparation method thereof, this method is that properties-correcting agent has prepared modification brown coal class fluid loss agent with urea, formaldehyde and phenol, and particularly a kind of have high temperature resistance ability and a high drilling fluid additive that falls filtration effect.
Background technology
Fluid loss agent is stable in order to guarantee property of drilling fluid; Reduce harmful liquid to the stratum leak-off; And the important additive for drilling fluid of stabilizing borehole, assurance hole diameter rule; From product category, additive for drilling fluid has begun from simplification compound, homopolymer to multipolymer, graft product development, from main use natural product to the modified natural production development; From the viewpoint of protection hydrocarbon zone, fluid loss agent is one type of very important in drilling fluid treatment agent; Collateral security is normally crept into, is reduced the drilling fluid maintenance service and reduces additive for drilling fluid consumption, and fluid loss agent also is indispensable one type of treatment agent in the drilling fluid.Filtrate reducer for drilling fluid involved in the present invention is that main raw material forms through the copolymerization of phenol urea-formaldehyde resin, grafting with the natural product brown coal promptly, has efficient heat and salinity tolerance ability.
Mostly filtrate reducer for drilling fluid commonly used at present is the natural or synthetic polymer that relative molecular weight is moderate, and though satisfied on-the-spot needs, also there are some problems in they when reducing drilling fluid filtration.For example product salt resistances such as sulfonated lignite resin SRC, high temperature fluid loss agent SPNH, sulfonated-pheno-formoldehyde resin SMP are not enough, though sulfonated lignite SMC can be used for fresh-water drilling fluid, and certain temperature resistance ability (the temperature resistance ability in fresh-water drilling fluid reaches 200～230 ℃) arranged; But saline-alkaline tolerance is no more than 3% (200 ℃); After salt and calcium contamination, the drilling fluid tackify falls filtration effect and obviously reduces; SMC and chromium-iron lignosulfonate are used, and can put forward the ability of high capability of anti-salt, calcium; Cooperate with arsenic and can improve the temperature resistance ability.Sulfonated-pheno-formoldehyde resin SMP is good heat resisting fluid loss reducing agent; Two kinds of models of SMP-1 and SMP-2 are arranged; Bubble seriously but have, improve the shortcoming of drilling fluid viscosity, and SMP-1 must be just obvious with the composite result of use of sulfonated lignite SMC; Though SMP-2 can be used for saturated salt-water drilling fluid, must be with it and sulfonated lignite SMC and the good effect of the composite use competence exertion of sulfonation tannin extract SMK.SMP-2 can replace SMP-1 in the unsaturated salt-water drilling fluid of high temperature resistance, and just dosage need be bigger than normal, and the irreplaceable SMP-2 of SMP-1 is used for saturated salt-water drilling fluid.The petroleum exploration and development paces are accelerated in recent years; Deep-well ultra deep well quantity rolls up; Temperature resistance, anti-salt property to treatment agent require increasingly high; So development novel anti high temperature, anti-salt, cheap fluid loss agent be for the progress and the success ratio that improve exploratory development, environment protection and economic benefit all have important in theory and practical significance even for the downhole safety of Oil-Gas Well Engineering, wellbore stability, oil layer protection.
Summary of the invention:
The preparation method who the purpose of this invention is to provide a kind of valchovite class heat and salinity tolerance fluid loss agent that uses as additive for drilling fluid.The main raw material of this fluid loss agent is brown coal; This preparation method adopts the not production process route of deslagging of single stage method; It is big to have production intensity, and raw material availability is high, does not form secondary pollution; The advantage that the heat and salinity tolerance performance is good can be applicable to widely that the deep drilling exploration under fresh water, the saline pollution uses.
A kind of filtrate reducer for drilling fluid is characterized in that, forms with sulfonated urea-formaldehyde and sulfonated phenolic hybrid resin modification brown coal, and proportioning raw materials is:
Brown coal: 10%-20%; Highly basic (NaOH, one kind of KOH or the two mixture): 2%-4%; Water: 50%-60%; Phenol: 2%-5.5%; Formaldehyde: 8%-15%; Urea: 3%-7%; Hydrolyzed acrylonitrile sodium salt: 0.15%-2%; SEPIGEL 305: 0.125%-0.5%; Sulphonating agent (S-WAT, sodium sulfite anhy 96, one or more mixtures in the Sodium Metabisulfite): 2%-7% all is weight percentage.
The preparation method of fluid loss agent of the present invention comprises the steps:
(1) in reaction kettle, adds phenol, formaldehyde (20wt%-40wt% of the total consumption of formaldehyde) and sulphonating agent (20wt%-35wt% of the total consumption of sulphonating agent), 55-70 ℃ of reaction 15-30 minute.
(2) add urea and formaldehyde (60wt%-80wt% of the total consumption of formaldehyde) and sulphonating agent (25wt%-40wt% of the total consumption of sulphonating agent) in the product of step (2), design temperature is 85-97 ℃, reacts 10 minutes.
(3) treat that temperature rises between 85-97 ℃, add poly hydrolyzate, add entry, highly basic and brown coal subsequently, reacted 30 minutes.
(4) add SEPIGEL 305 and sulphonating agent (25wt%-55wt% of the total consumption of sulphonating agent), reacted then 1.5-4 hour, the feed liquid that obtains promptly gets the fluid loss agent product through drying and crushing.
The application of fluid loss agent according to the invention, Applicable temperature generally in room temperature to 210 ℃, can in water mud and salty mud, use.
Fluid loss agent of the present invention is applicable to the leak-off effect of falling of water mud and salty mud.Establishing criteria Q/SH10201881-2008 estimates.To test with sodium soil, water, soda ash light and mix 20min,, promptly get basic slurry airtight maintenance 24 hours in 8: 100: 0.25 ratio high speed (10000 rev/mins).
Get two parts of bases slurries 400ml that prepare, add the 12.0g sample respectively, high-speed stirring 20min, a copy of it airtight maintenance 16 hours under room temperature, high-speed stirring 5min measures press filtration vector in the 30min room temperature; Another part adds digestion tank, rolling 16h under 180 ℃ of aging temperatures, and cooling is taken out, high-speed stirring 5min, the high temperature and high pre ssure filtration of fresh water slurry behind the mensuration high temperature ageing (150 ℃, 3.45MPa).
Get two parts of base slurry 400ml that prepare, add sodium-chlor (pressing the brine concentration of being surveyed adds) respectively, high-speed stirring 20min; Adding the 20.0g sample respectively, high-speed stirring 20min, the digestion tank of packing into; Rolling 16h under 180 ℃ of aging temperatures, cooling is taken out, high-speed stirring 5min; Middle press filtration vector after mensuration wears out respectively and high temperature and high pre ssure filtration (150 ℃, 3.45MPa).
This patent mainly is raw material with brown coal, because the humic acid molecule in the brown coal is to be made up of with various active functional group many cyclophane nuclears, has multiple functional group; The wetting ability of molecule, complex ability and absorption dispersive ability are stronger, think the basis that modification provides, through the modification of urea-formaldehyde resin; Improve temperature resistance, the saline-alkaline tolerance of modified product, the modified product phenomenon of in application process, not bubbling also have good viscosity-reducing performance simultaneously because the existence of urea-formaldehyde resin makes; Overcome phenolic resin modified product foaming and put forward sticking shortcoming; And modified product has biodegradable, is ep-type material, as having a extensive future of additive for drilling fluid.
Embodiment:
Following embodiment is to further specify of the present invention, but the present invention is not limited thereto.
Embodiment 1:
Measure 10ml phenol with graduated cylinder, 13ml formaldehyde adds in the 500ml there-necked flask, is warming up to more than 60 ℃, adds the 3.4g Sodium Metabisulfite; Reaction 30min, the back adds 10.7g urea, 23ml formaldehyde, 3.4g Sodium Metabisulfite; Begin to heat up, be warming up to and add 10g poly hydrolyzate (self-control, reference [1], as follows) more than 90 ℃; Reaction 5min adds sodium hydroxide solution (200ml zero(ppm) water, dissolving 12g sodium hydroxide), adds 60g brown coal (humic acids content >=60%) subsequently; Reacted 30 minutes, and added the 9g Sodium Metabisulfite, the 1g SEPIGEL 305.Reaction 2-3.5h takes out cooling, and oven dry is pulverized and obtained product A.
Embodiment 2:
Measure 11ml phenol with graduated cylinder, 11ml formaldehyde adds in the 500ml there-necked flask, is warming up to 60 ℃, adds the 3.67g Sodium Metabisulfite; Reaction 30min, the back adds 11.73g urea, 25.0ml formaldehyde; 3.67g Sodium Metabisulfite begins to heat up, and adds 10g poly hydrolyzate (self-control) after being warming up to 90 ℃; Reaction 5min adds sodium hydroxide solution (200ml zero(ppm) water, dissolving 12g sodium hydroxide), adds 60g brown coal (humic acids content >=60%) subsequently; Reacted 30 minutes, and added the 9g Sodium Metabisulfite, the 1g SEPIGEL 305.Reaction 2-3.5h takes out cooling, and oven dry is pulverized and obtained product B.
Embodiment 3:
Measure 12ml phenol with graduated cylinder, 12ml formaldehyde adds in the 500ml there-necked flask, is warming up to 60 ℃, adds the 4g Sodium Metabisulfite; Reaction 30min, the back adds 12.8g urea, 28ml formaldehyde; The 4g Sodium Metabisulfite begins to heat up, and adds 10g poly hydrolyzate (self-control) after being warming up to 90 ℃; Reaction 5min adds sodium hydroxide solution (200ml zero(ppm) water, dissolving 12g sodium hydroxide), adds 60g brown coal (humic acids content >=60%) subsequently; Reacted 30 minutes, and added the 9g Sodium Metabisulfite, the 1g SEPIGEL 305.Reaction 2-3.5h takes out cooling, and oven dry is pulverized and obtained products C.
Embodiment 4:
Measure 13ml phenol with graduated cylinder, 13ml formaldehyde adds in the 500ml there-necked flask, is warming up to 60 ℃, adds the 4.33g Sodium Metabisulfite; Reaction 30min, the back adds 13.87g urea, 30.ml formaldehyde; 4.33g Sodium Metabisulfite begins to heat up, and adds 10g poly hydrolyzate (self-control) after being warming up to 90 ℃; Reaction 5min adds sodium hydroxide solution (200ml zero(ppm) water, dissolving 12g sodium hydroxide), adds 60g brown coal (humic acids content >=60%) subsequently; Reacted 30 minutes, and added the 9g Sodium Metabisulfite, the 1g SEPIGEL 305.Reaction 2-3.5h takes out cooling, and oven dry is pulverized and obtained product D.
Embodiment 5:
Measure 15ml phenol with graduated cylinder, 15ml formaldehyde adds in the 500ml there-necked flask, is warming up to 60 ℃, adds the 5g Sodium Metabisulfite; Reaction 30min, the back adds 16g urea, 35ml formaldehyde; The 5g Sodium Metabisulfite begins to heat up, and adds 7g poly hydrolyzate (self-control) after being warming up to 90 ℃; Reaction 5min adds sodium hydroxide solution (200ml zero(ppm) water, dissolving 12g sodium hydroxide), adds 60g brown coal (humic acids content >=60%) subsequently; Reacted 30 minutes, and added the 9g Sodium Metabisulfite, the 1g SEPIGEL 305.Reaction 2-3.5h takes out cooling, and oven dry is pulverized and obtained product E.
Embodiment 6:
Measure 15ml phenol with graduated cylinder, 15ml formaldehyde adds in the 500ml there-necked flask, is warming up to 60 ℃, adds the 5g Sodium Metabisulfite; Reaction 30min, the back adds 16g urea, 35ml formaldehyde; The 5g Sodium Metabisulfite begins to heat up, and adds 7g poly hydrolyzate (self-control) after being warming up to 90 ℃; Reaction 5min adds sodium hydroxide solution (250ml zero(ppm) water, dissolving 15g sodium hydroxide), adds 80g brown coal (humic acids content >=60%) subsequently; Reacted 30 minutes, and added the 10g Sodium Metabisulfite, the 1g SEPIGEL 305.Reaction 2-3.5h takes out cooling, and oven dry is pulverized and obtained product F.
Embodiment 7:
Measure 15ml phenol with graduated cylinder, 20ml formaldehyde adds in the 500ml there-necked flask, is warming up to 60 ℃, adds the 5g Sodium Metabisulfite; Reaction 30min, the back adds 16g urea, 35ml formaldehyde; The 5g Sodium Metabisulfite begins to heat up, and adds 7g poly hydrolyzate (self-control) after being warming up to 90 ℃; Reaction 5min adds sodium hydroxide solution (250ml zero(ppm) water, dissolving 15g sodium hydroxide), adds 80g brown coal (humic acids content >=60%) subsequently; Reacted 30 minutes, and added the 9g Sodium Metabisulfite, the 1g SEPIGEL 305.Reaction 2-3.5h takes out cooling, and oven dry is pulverized and obtained product G.
Embodiment 8:
Measure 15ml phenol with graduated cylinder, 15ml formaldehyde adds in the 500ml there-necked flask, is warming up to 60 ℃; Add the 5g Sodium Metabisulfite, reaction 30min, the back adds 16g urea; 35ml formaldehyde, the 5g Sodium Metabisulfite begins to heat up; Add the 7g poly hydrolyzate after being warming up to 90 ℃, reaction 5min adds brown coal (humic acids content >=60%) alkali lye (normal temperature is down with 5.66%, and the sodium hydroxide solution of 200ml dissolves the brown coal alkali lye that the 60g brown coal make); Reacted 30 minutes, and added the 9g Sodium Metabisulfite, the 1g SEPIGEL 305.Reaction 3-4h takes out cooling, and oven dry is pulverized and obtained product H.
Embodiment 9:
Measure 15ml phenol with graduated cylinder, 20ml formaldehyde adds in the 500ml there-necked flask, is warming up to 60 ℃; Add the 5g Sodium Metabisulfite, reaction 30min, the back adds 16g urea; 35ml formaldehyde, the 5g Sodium Metabisulfite begins to heat up; Add the 4g poly hydrolyzate after being warming up to 90 ℃, reaction 5min adds brown coal (humic acids content >=60%) alkali lye (normal temperature is down with 5.66%, and the sodium hydroxide solution of 200ml dissolves the brown coal alkali lye that the 60g brown coal make); Reacted 30 minutes, and added the 9g Sodium Metabisulfite, the 1g SEPIGEL 305.Reaction 3-4h takes out cooling, and oven dry is pulverized and obtained product I.
Embodiment 10:
Measure 15ml phenol with graduated cylinder, 15ml formaldehyde adds in the 500ml there-necked flask, is warming up to 60 ℃; Add the 5g Sodium Metabisulfite, reaction 30min, the back adds 16g urea; 35ml formaldehyde, the 5g Sodium Metabisulfite begins to heat up; Add the 7g poly hydrolyzate after being warming up to 90 ℃, reaction 5min adds brown coal (humic acids content >=60%) alkali lye (normal temperature is down with 5.66%, and the sodium hydroxide solution of 200ml dissolves the brown coal alkali lye that the 60g brown coal make); Reacted 30 minutes, and added the 9g Sodium Metabisulfite.Reaction 3-4h takes out cooling, and oven dry is pulverized and obtained product J.
The 4% salt solution vector evaluation result of above-mentioned sample A～K is shown in table 1 (testing method adopts the Q/SH10201881-2008 standard, and is as follows).
The different sample filter loss contrasts of table 1.
The fresh water slurry evaluation result of above-mentioned sample A～K is shown in table 2.
The different sample filter loss contrasts of table 2.
Reference:
[1] Liu Yuqing, Sun Jinsheng, Wang Shuqi, etc. the synthetic and application [J] of high-temperature resisting and salt-resisting positively charged ion fluid loss agent CHSP-I. oilfield chemistry, 1996,13 (1): 21～24.
Claims (5)
1. a filtrate reducer for drilling fluid is characterized in that, forms with sulfonated urea-formaldehyde and sulfonated phenolic hybrid resin modification brown coal, and proportioning raw materials is:
Brown coal: 10%-20%; Highly basic 2%-4%; Water 50%-60%; Phenol: 2%-5.5%; Formaldehyde: 8%-15%; Urea: 3%-7%; Hydrolyzed acrylonitrile sodium salt: 0.15%-2%; SEPIGEL 305: 0.125%-0.5%, sulphonating agent: 2%-7% all is weight percentage.
2. filtrate reducer for drilling fluid as claimed in claim 1 is characterized in that, said highly basic is NaOH, one kind of KOH or the two mixture.
3. filtrate reducer for drilling fluid as claimed in claim 1 is characterized in that, said sulphonating agent is a S-WAT, sodium sulfite anhy 96, one or more mixtures in the Sodium Metabisulfite.
4. like the preparation method of each described fluid loss agent of claim 1～3, comprise the steps:
(1) in reaction kettle, adds phenol, formaldehyde and sulphonating agent, 55-70 ℃ of reaction 15-30 minute.
(2) add urea and formaldehyde and sulphonating agent in the product of step (2), design temperature is 85-97 ℃, reacts 10 minutes.
(3) treat that temperature rises between 85-97 ℃, add poly hydrolyzate, add entry, highly basic and brown coal subsequently, reacted 30 minutes.
(4) add SEPIGEL 305 and sulphonating agent, reacted then 1.5-4 hour, the feed liquid that obtains promptly gets the fluid loss agent product through drying and crushing.
5. like the application of each described fluid loss agent of claim 1～3, Applicable temperature is in room temperature to 210 ℃, use in water mud and salty mud.
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| CN103666415A (en) * | 2013-12-23 | 2014-03-26 | 河南海洋化工有限公司 | Efficient temperature resistance fluid loss agent for drilling fluid and preparation method thereof |
| CN103772558A (en) * | 2014-01-20 | 2014-05-07 | 齐鲁工业大学 | Preparation method of low-viscosity hydrolyzed polyacrylonitrile sodium salt filtrate reducer |
| CN103849361A (en) * | 2014-02-13 | 2014-06-11 | 克拉玛依友联实业有限责任公司 | High-temperature resistant anti-collapse blocking agent and preparation method thereof |
| CN104559984A (en) * | 2013-10-29 | 2015-04-29 | 中国石油化工股份有限公司 | Composition capable of decreasing viscosity of hydrocarbon oil and method for decreasing viscosity of hydrocarbon oil |
| CN104910330A (en) * | 2015-06-16 | 2015-09-16 | 北京中科天启油气技术有限公司 | High-density fluid loss additive for drilling fluids and preparation method thereof |
| CN107011803A (en) * | 2017-04-20 | 2017-08-04 | 中国石油化工股份有限公司 | A kind of sulfonation tannin extract and preparation method thereof |
| CN107779177A (en) * | 2016-08-24 | 2018-03-09 | 中石化石油工程技术服务有限公司 | Clay inhibition high temperature resistance lignite class fluid loss additive and preparation method thereof |
| CN108018028A (en) * | 2017-12-14 | 2018-05-11 | 玉门油田科达化学有限责任公司 | A kind of drilling fluid walchowite and its production technology |
| CN110093007A (en) * | 2019-05-05 | 2019-08-06 | 中国石油化工股份有限公司 | The method of modifying of the quick slip casting bag-type blockage quick-set of oil pipeline |
| CN110105706A (en) * | 2019-05-05 | 2019-08-09 | 中国石油化工股份有限公司 | A kind of quick-set for the quick slip casting bag-type blockage of oil pipeline |
| CN110483795A (en) * | 2019-08-23 | 2019-11-22 | 广东方中高新材料有限公司 | A kind of supermolecule sulfonated phenolic condensation polymer and its preparation method and application |
| CN111500269A (en) * | 2020-06-08 | 2020-08-07 | 保定市三拓化工产品有限公司 | Drilling fluid filtrate reducer |
| CN116355599A (en) * | 2023-06-01 | 2023-06-30 | 四川巨正科技有限公司 | Environment-friendly lignite resin for drilling fluid and preparation method thereof |
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| CN104559984A (en) * | 2013-10-29 | 2015-04-29 | 中国石油化工股份有限公司 | Composition capable of decreasing viscosity of hydrocarbon oil and method for decreasing viscosity of hydrocarbon oil |
| CN103666415A (en) * | 2013-12-23 | 2014-03-26 | 河南海洋化工有限公司 | Efficient temperature resistance fluid loss agent for drilling fluid and preparation method thereof |
| CN103772558A (en) * | 2014-01-20 | 2014-05-07 | 齐鲁工业大学 | Preparation method of low-viscosity hydrolyzed polyacrylonitrile sodium salt filtrate reducer |
| CN103849361A (en) * | 2014-02-13 | 2014-06-11 | 克拉玛依友联实业有限责任公司 | High-temperature resistant anti-collapse blocking agent and preparation method thereof |
| CN104910330A (en) * | 2015-06-16 | 2015-09-16 | 北京中科天启油气技术有限公司 | High-density fluid loss additive for drilling fluids and preparation method thereof |
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| CN108018028A (en) * | 2017-12-14 | 2018-05-11 | 玉门油田科达化学有限责任公司 | A kind of drilling fluid walchowite and its production technology |
| CN110093007A (en) * | 2019-05-05 | 2019-08-06 | 中国石油化工股份有限公司 | The method of modifying of the quick slip casting bag-type blockage quick-set of oil pipeline |
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| CN110105706B (en) * | 2019-05-05 | 2021-11-05 | 中国石油化工股份有限公司 | Quick setting material for quick grouting bag type plugging of oil pipeline |
| CN110483795A (en) * | 2019-08-23 | 2019-11-22 | 广东方中高新材料有限公司 | A kind of supermolecule sulfonated phenolic condensation polymer and its preparation method and application |
| CN111500269A (en) * | 2020-06-08 | 2020-08-07 | 保定市三拓化工产品有限公司 | Drilling fluid filtrate reducer |
| CN111500269B (en) * | 2020-06-08 | 2022-06-28 | 保定市三拓化工产品有限公司 | Filtrate reducer for drilling fluid |
| CN116355599A (en) * | 2023-06-01 | 2023-06-30 | 四川巨正科技有限公司 | Environment-friendly lignite resin for drilling fluid and preparation method thereof |
| CN116355599B (en) * | 2023-06-01 | 2023-08-08 | 四川巨正科技有限公司 | Environment-friendly lignite resin for drilling fluid and preparation method thereof |
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Application publication date: 20120411 |