CN104140509A - Preparation method for sulfonated-phenol-formaldehyde resin formed by modifying benzoxazine resin - Google Patents
Preparation method for sulfonated-phenol-formaldehyde resin formed by modifying benzoxazine resin Download PDFInfo
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- CN104140509A CN104140509A CN201410365369.2A CN201410365369A CN104140509A CN 104140509 A CN104140509 A CN 104140509A CN 201410365369 A CN201410365369 A CN 201410365369A CN 104140509 A CN104140509 A CN 104140509A
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Abstract
A preparation method for sulfonated-phenol-formaldehyde resin formed by modifying benzoxazine resin includes the steps that (1), bisphenol A type benzoxazine with the particle size smaller than or equal to 25 mm is pulverized to be powder through a pulverizing machine, wherein the particle size of the powder is 10 micrometers-125 micrometers, and the powder is standby; (2), the powder obtained in the step (1) and modified sulfonated phenolic resin agents are thrown into a reaction kettle according to the mass ratio of 1:20, mixed, stirred for one hour at the temperature of 105 DEG C and then delivered into an ultrasonic emulsifying device through a discharging pump to be ultrasonically emulsified for 20 minutes to obtain a mixed solution, and the mixed solution is standby; (3), spraying drying is performed on the mixed solution in the step (2) to obtain the modified sulfonated-phenol-formaldehyde resin. The sulfonated-phenol-formaldehyde resin can be resistant to high temperature of 200 DEG C, has an obvious effect of lowering the filter loss of drilling fluid and can meet the requirements for three high well drilling.
Description
Technical field
The present invention relates to a kind of preparation method of the novel sulfonated-pheno-formoldehyde resin SMP-of the hyperconcentration type III forming with benzoxazine colophony modification.
Background technology
Sulfonated phenol formaldehyde resin is a kind of temperature resistance, the salt resistant filter loss reduction agent that the seventies, China scientific worker developed, its maximum feature is to utilize high temperature to carry out stress efficacy, thereby becomes an indispensable part in current domestic most deep drilling liquid system.But the sulfonated phenol formaldehyde resin service efficiency that at present production technique is produced is low, and inhibition is poor, in dark, shallow well section result of use is poor, can not meet salt solution and the control of saturated salt-water drilling fluid high temperature and high pre ssure filtration and rheological needs under ultra-high temperature condition.Sulfonated phenolic resin SMP-the II of " patent No.: 201010274133.X, patent name: a kind of preparation method of modified sulfomethal phenolaldehy resin for drilling liquid " described product Xi Wo company independent research, in its drilling fluid, anti-salt reaches 15%; Temperature resistance reaches 180 DEG C, has improved to a certain extent service efficiency, has played anti-salt temperature resistance and fall the effect of leak-off.But the demand that can't meet three Gao Jing (super dark, ultrahigh-temperature, ultra-high voltage) drilling well, it is under the condition that exceedes 180 DEG C, and as do not reached job requirements under the condition of 200 DEG C completely, and addition is larger, and client's drilling cost is higher.
Summary of the invention
In view of above-mentioned deficiency, the invention provides a kind of sulfonated-pheno-formoldehyde resin preparation method who forms with benzoxazine colophony modification, the modification sulfonated-pheno-formoldehyde resin (SMP-III) that the method is prepared, can further widen use range, high temperature resistant property is strong simultaneously, and temperature resistance reaches 200 DEG C, antisaturation salt solution, use the half that addition is my house journal's product (patent No.: 201010274133.X) sulfonated phenolic SMP-II, reduced client's drilling cost.
In order to achieve the above object, the present invention has adopted following technical scheme:
A sulfonated-pheno-formoldehyde resin preparation method who forms with benzoxazine colophony modification, concrete steps are as follows:
(1) granularity≤25mm bisphenol A-type benzoxazine is worn into the powder of granularity 10um-125um with pulverizing mill, for subsequent use;
(2) by step (1) gained powder and the modification sulphonation resol agent ratio input reactor of 1:20 in mass ratio, 105 DEG C of mix and blends were sent into ultrasonic emulsification device by discharging pump after 1 hour, and excusing from death emulsification 20 minutes, obtains mixed solution, for subsequent use;
(3) mixed solution of step (2) is sprayed and is dried, obtain sulfonated-pheno-formoldehyde resin of the present invention.
The agent of described modification sulphonation resol is made by following preparation method:
1. 1 mole of 1 mole of phenol, formaldehyde is added successively in the reactor with the reflux cooler of stirrer, 119 DEG C are stirred 10 minutes, cooling, maintain the temperature at 109 DEG C, then add successively 1 mole, formaldehyde, 0.5 mole of Sodium Pyrosulfite, water 40ml as sulphonating agent, the sulfonation time is 3 hours, finally adds 1 moles of formaldehyde, back flow reaction 3-4 hour at 97 DEG C-104 DEG C;
2. when reaction finishes, cooling, be cooled to 60 DEG C of-70 DEG C of dischargings, obtain the agent of modification sulphonation resol.
Preparation principle of the present invention: by ultrasonic wave, bisphenol A-type benzoxazine colophony and patented product (patent No.: 201010274133.X) modification sulphonation resol SMP-II are mixed into emulsion, make it to form multipolymer.
Energy high temperature resistance of the present invention reaches 200 DEG C, and the filter loss of drilling fluid is had to obvious reducing effect, can meet the requirement of three high well probings.
Saline-alkaline tolerance of the present invention is strong, can reach 30% pollution for anti-salt, can in nearly saturated salt-water drilling fluid, keep low filtration loss and the good mobility of drilling fluid, is a kind of desirable high temperature fluid loss agent.
Embodiment
A kind of sulfonated-pheno-formoldehyde resin preparation method who forms with benzoxazine colophony modification is as follows:
(1) preparation of powder: granularity≤25mm bisphenol A-type benzoxazine is worn into the powder of granularity 10um-125um with pulverizing mill, for subsequent use;
(2) preparation of modification sulphonation resol agent:
1. 1 mole of 1 mole of phenol, formaldehyde is added successively in the reactor with the reflux cooler of stirrer, 119 DEG C are stirred 10 minutes, cooling, maintain the temperature at 109 DEG C, then add successively 1 mole, formaldehyde, 0.5 mole of Sodium Pyrosulfite, water 40ml as sulphonating agent, the sulfonation time is 3 hours, finally adds 1 moles of formaldehyde, back flow reaction 3-4 hour at 97 DEG C-104 DEG C;
2. when reaction finishes, cooling, be cooled to 60 DEG C of-70 DEG C of dischargings, obtain the agent of modification sulphonation resol.
(3) by the modification sulphonation resol agent of step (1) gained powder and step (2) the gained ratio input reactor of 1:20 in mass ratio, 105 DEG C of mix and blends were sent into ultrasonic emulsification device by discharging pump after 1 hour, excusing from death emulsification 20 minutes, obtains mixed solution, for subsequent use;
(4) mixed solution of step (3) is sprayed and is dried, obtain sulfonated-pheno-formoldehyde resin of the present invention.
Beneficial effect of the present invention refers to table 1-table 4.
Table 1 is technical indicator of the present invention, impact on drilling fluid rheology and temperature resistance, salt resistance, high temperature and high pre ssure filtration etc.
The technology contrast of product of the present invention and patented product (patent No. 201010274133.X) modification sulphonation resol SMP-II (hereinafter to be referred as SMP-II) refers to table 2-table 4.
Table 2 the present invention and SMP-II temperature resistance simultaneous test table.
Table 3 the present invention and SMP-II salt resistance simultaneous test table.
The impact on drilling fluid rheology in drilling fluid system of table 4 the present invention and SMP-II.
As can be seen from Table 4, under equal conditions, reach identical result of use, addition of the present invention is only the half of SMP-II.
Claims (3)
1. a sulfonated-pheno-formoldehyde resin preparation method who forms with benzoxazine colophony modification, is characterized in that this preparation method's concrete steps are as follows:
(1) granularity≤25mm bisphenol A-type benzoxazine is worn into the powder of granularity 10um-125um with pulverizing mill, for subsequent use;
(2) by step (1) gained powder and the modification sulphonation resol agent ratio input reactor of 1:20 in mass ratio, 105 DEG C of mix and blends were sent into ultrasonic emulsification device by discharging pump after 1 hour, and excusing from death emulsification 20 minutes, obtains mixed solution, for subsequent use;
(3) mixed solution of step (2) is sprayed and is dried, obtain modification sulfonated-pheno-formoldehyde resin.
2. preparation method according to claim 1, is characterized in that: the agent of described modification sulphonation resol is made by following preparation method:
1. 1 mole of 1 mole of phenol, formaldehyde is added successively in the reactor with the reflux cooler of stirrer, 119 DEG C are stirred 10 minutes, cooling, maintain the temperature at 109 DEG C, then add successively 1 mole, formaldehyde, 0.5 mole of Sodium Pyrosulfite, water 40ml as sulphonating agent, the sulfonation time is 3 hours, finally adds 1 moles of formaldehyde, back flow reaction 3-4 hour at 97 DEG C-104 DEG C;
2. when reaction finishes, cooling, be cooled to 60 DEG C of-70 DEG C of dischargings, obtain sulfonated phenol formaldehyde resin agent.
3. one kind by the prepared sulfonated-pheno-formoldehyde resin of preparation method described in claim 1 or 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410365369.2A CN104140509B (en) | 2014-07-29 | 2014-07-29 | A kind of with the sulfonated-pheno-formoldehyde resin preparation method of benzoxazine colophony modification |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410365369.2A CN104140509B (en) | 2014-07-29 | 2014-07-29 | A kind of with the sulfonated-pheno-formoldehyde resin preparation method of benzoxazine colophony modification |
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| CN104140509A true CN104140509A (en) | 2014-11-12 |
| CN104140509B CN104140509B (en) | 2015-11-04 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104788634A (en) * | 2015-05-08 | 2015-07-22 | 天津中油渤星工程科技有限公司 | Preparation method of high-temperature-resistant modified sulfonated phenol formaldehyde resin for drilling fluids |
| CN111925780A (en) * | 2020-10-15 | 2020-11-13 | 山东科兴化工有限责任公司 | Preparation method of high-temperature-resistant high-strength plugging agent for plugging of oil and gas well |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033391A (en) * | 2006-12-29 | 2007-09-12 | 赵立勋 | Method of preparing sulfonated-phenoformoldehyde resin for drilling fluid |
| CN102241804A (en) * | 2011-05-12 | 2011-11-16 | 四川上之登新材料有限公司 | Preparation method of coupling phenolic resin used for drilling fluid |
-
2014
- 2014-07-29 CN CN201410365369.2A patent/CN104140509B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033391A (en) * | 2006-12-29 | 2007-09-12 | 赵立勋 | Method of preparing sulfonated-phenoformoldehyde resin for drilling fluid |
| CN102241804A (en) * | 2011-05-12 | 2011-11-16 | 四川上之登新材料有限公司 | Preparation method of coupling phenolic resin used for drilling fluid |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104788634A (en) * | 2015-05-08 | 2015-07-22 | 天津中油渤星工程科技有限公司 | Preparation method of high-temperature-resistant modified sulfonated phenol formaldehyde resin for drilling fluids |
| CN104788634B (en) * | 2015-05-08 | 2017-11-07 | 天津中油渤星工程科技有限公司 | A kind of preparation method of drilling fluid high temperature resistance modification sulphonation phenolic resin |
| CN111925780A (en) * | 2020-10-15 | 2020-11-13 | 山东科兴化工有限责任公司 | Preparation method of high-temperature-resistant high-strength plugging agent for plugging of oil and gas well |
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| CN104140509B (en) | 2015-11-04 |
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Address after: Section 2, Shenzhen Road East, Guanghan Economic Development Zone, Deyang City, Sichuan Province Patentee after: Sichuan Zhengrong shangzhideng Technology Co.,Ltd. Address before: Section 2, Shenzhen Road East, Guanghan Economic Development Zone, Deyang City, Sichuan Province Patentee before: SICHUAN SHANGZHIDENG NEW MATERIAL Co.,Ltd. |
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Effective date of registration: 20210412 Address after: No.3, section 3, East Shenzhen road, Guanghan City, Deyang City, Sichuan Province Patentee after: SICHUAN ZHENGRONG IND Co.,Ltd. Patentee after: Sichuan Zhengrong shangzhideng Technology Co.,Ltd. Address before: Section 2, Shenzhen Road East, Guanghan Economic Development Zone, Deyang City, Sichuan Province Patentee before: Sichuan Zhengrong shangzhideng Technology Co.,Ltd. |
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Address after: No.3, section 3, East Shenzhen road, Guanghan City, Deyang City, Sichuan Province Patentee after: Sichuan Zhengrong Industrial Co.,Ltd. Patentee after: Sichuan shangzhideng New Material Technology Co., Ltd Address before: No.3, section 3, East Shenzhen road, Guanghan City, Deyang City, Sichuan Province Patentee before: Sichuan Zhengrong Industrial Co.,Ltd. Patentee before: Sichuan Zhengrong shangzhideng Technology Co., Ltd |
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