CN100595254C - Method for preparing amphoteric ion polymer fluid loss additive - Google Patents
Method for preparing amphoteric ion polymer fluid loss additive Download PDFInfo
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- CN100595254C CN100595254C CN200810047241A CN200810047241A CN100595254C CN 100595254 C CN100595254 C CN 100595254C CN 200810047241 A CN200810047241 A CN 200810047241A CN 200810047241 A CN200810047241 A CN 200810047241A CN 100595254 C CN100595254 C CN 100595254C
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- mixed solution
- fluid loss
- ion polymer
- amphoteric ion
- loss additive
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Abstract
The invention relates to a process for preparing amphoteric ion polymer fluid loss additive, which is characterized in that the process for preparation comprises the following steps: firstly, dissolving acrylamide and 2- acryloylamino-2-methylpropanesulfonic acid into water according to the mass ratio which is 10:1-3:1, getting mixed solution A, secondly, leading the mixed solution A to react 3-6hunder the temperature which is 35 DEG C to 70 DEF C, and pH value which is 3-10 and under the condition of adding with initiating agent, and getting mixed solution B, thirdly, cooling the mixed solution B with ice-water bath, adding NaClO which is -10 DEG C-5 DEG C and contains NaOH according to the substance ratio which is -CONH2:NaClO: NaOH=1:0.1:10-1:1:10, reacting 5-10h in ice-water bath, getting mixed solution C, fourthly, adding HCl solution, and getting viscous products, fifthly, stirring and washing viscous products in carbinol to get white sediment, and then taking out sediment, granulating, drying, disintegrating, and then getting products. The process for preparation has the advantages of high-temperature resistance, salinity tolerance and low production cost, and the conditionof the process is moderate and controllable.
Description
Technical field
The present invention relates to a kind of preparation method of amphoteric ion polymer fluid loss additive.
Background technology
Fluid loss agent is to guarantee that property of drilling fluid is stable, minimizing is harmful to the important additive for drilling fluid of liquid to stratum leak-off, stabilizing borehole and assurance hole diameter rule.Along with the development of oil drilling and the increase of deep-well marine drilling project, the requirement of filtrate reducer for drilling fluid is also improved constantly, (NaCl content is greater than 10%, CaCl to satisfy salt tolerance
2Content is greater than 5%) and the new demand of high temperature resistance (temperature is higher than 150 ℃).Fluid loss agent at present commonly used is as pregelatinized Starch, polyoxyethylene non-ionic type fluid loss agents such as (PEO), anionic fluid loss agents such as modified-cellulose class (CMC), modified starch series (CMS), hydrolyzed polyacrylonitrile class (HPAN), hydro-polyacrylamide class (HPAM), sulfonation series products can not satisfy this requirement fully.Therefore developing high temperature resistance salt tolerant fluid loss agent is the focus of studying at present.Mainly contain three kinds of methods: (1) carries out modification to the propylene copolymers fluid loss agent; (2) serve as basis and other its monomer synthetic multipolymers with 2-acrylamido-2-methyl propane sulfonic acid (AMPS); (3) exploitation amphoteric ion polymer class fluid loss agent.Because amphoteric ion polymer fluid loss additive has expansion, the dispersion that suppresses shale in addition, therefore the effect of stabilizing borehole receives much attention.At present the method for synthetic amphoteric ion polymer class fluid loss agent mainly is to be principal monomer with acrylamide (AM) and 2-acrylamido-2-methyl propane sulfonic acid (AMPS), being aided with other cationic monomer (being mainly quaternary ammonium salt) again comes synthetic, although good filtration effect and the high temperature resistance salt resistance ability of falling arranged, but synthesis condition is wayward, and cationic monomer is all very expensive.So suitability for industrialized production and practical application all have suitable difficulty.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of high temperature resistance, salt tolerant, amphoteric ion polymer fluid loss additive that cost is low, this method mild condition is controlled.
To achieve these goals, technical scheme of the present invention is: a kind of preparation method of amphoteric ion polymer fluid loss additive is characterized in that it comprises the steps:
1) mass ratio by acrylamide and 2-acrylamido-2-methyl propane sulfonic acid is 10: 1~3: 1, is dissolved in the water, and gets mixed solution A, and the mass concentration of mixed solution A is 8%~30%;
2) mixed solution A is at 35 ℃~70 ℃, and pH value 3~10 adds under the initiator condition, and reaction 3~6h gets mixing solutions B, and wherein, initiator is 0.1%~1% of acrylamide and 2-acrylamido-2-methyl propane sulfonic acid quality;
3) mixing solutions B cools off with ice-water bath, treat temperature-stable after, by-CONH
2: NaClO: NaOH=1: 0.1: 10~1: 1: 10 amount adds than (being mol ratio) and contains NaOH-10 ℃~5 ℃ NaCl0 solution, reacts 5~10h in the ice-water bath, gets mixed solution C;
4) then by HCl: NaOH=1: 1 amount adds HCl solution than (being mol ratio), must glue the shape product;
5) sticking shape product agitator treating in methyl alcohol gets the pale precipitation thing, takes out throw out pelletizing, oven dry, pulverizing then and promptly gets the amphoteric ion polymer fluid loss additive product.
Described acrylamide (AM) adopts technical grade product, and Tianjin Kermel Chemical Reagent Co., Ltd. produces.
Described 2-acrylamido-2-methyl propane sulfonic acid (AMPS) adopts technical grade product, and extra large chemical industry company limited produces in Juye County, Shandong Province.
Described initiator is an ammonium persulphate; Perhaps be ammonium persulphate and sodium bisulfite, the mass ratio of ammonium persulphate and sodium bisulfite is 2: 1; Ammonium persulphate, sodium bisulfite are analytical pure, and Chemical Reagent Co., Ltd., Sinopharm Group produces.
Described chlorine bleach liquor is analytical pure (available chlorine content>10%), and Jin Bei Fine Chemical Co., Ltd in Tianjin produces.
Above-mentioned amphoteric ion polymer fluid loss additive product is used for fresh water, salt solution, saturated brine, compound salt solution or calcic salt-water drilling fluid, excellent filtration reduction energy is all arranged.When its consumption was 1.0% (quality), the API fluid loss that can make the calcic salt-water drilling fluid was reduced to 10mL from the 170mL of base slurry; Through 180 ℃ of aging 16h that roll, fluid loss only is 13ml, and high temperature resistance, salt resistance ability are strong.
The invention has the beneficial effects as follows:
1, the cation group (NH in the amphoteric ion polymer fluid loss additive of the present invention
3 +) can strengthen the absorption of fluid loss agent on the clay surface ,-NH
3 +Can snap in the mesh in the clay lattice, increase the probability that the fluid loss agent molecule stops up pore; Anionic group (SO in this fluid loss agent
3 -) saline-alkaline tolerance is strong, thereby strengthen its filtration reduction energy under high temperature and high salt concentration.
2, method of the present invention, its mild condition is controlled, the product yield height, favorable reproducibility, do not need expensive cationic monomer [the present invention adopts source abundant acrylamide (AM) and 2-acrylamido-2-methyl propane sulfonic acid (AMPS), and cost is low], the industrialization production feasibility height.Therefore higher actual application ability and market outlook are arranged.
Embodiment
Embodiment 1:
A kind of preparation method of amphoteric ion polymer fluid loss additive, it comprises the steps:
1) mass ratio by acrylamide (AM) and 2-acrylamido-2-methyl propane sulfonic acid (AMPS) is 10: 1, is dissolved in the water, and gets mixed solution A, and the mass concentration of mixed solution A is 8%;
2) mixed solution A is at 35 ℃, and pH value 3 adds under the initiator condition, and reaction 3h gets mixing solutions B, and wherein, initiator is 0.1% of acrylamide and 2-acrylamido-2-methyl propane sulfonic acid (AM and AMPS) quality;
3) mixing solutions B cools off with ice-water bath, treat temperature-stable after, by-CONH
2(amido): NaClO: NaOH=1: 0.1: 10 amount adds than (being mol ratio) and contains NaOH-10 ℃ NaClO solution, reacts 5h in the ice-water bath, gets mixed solution C;
4) then by HCl: NaOH=1: 1 amount slowly adds HCl solution than (being mol ratio), must glue the shape product;
5) sticking shape product in methyl alcohol repeatedly agitator treating get the pale precipitation thing, take out throw out pelletizing, oven dry, pulverizing then and promptly get amphoteric ion polymer fluid loss additive product (yellow powder powder).
Described acrylamide (AM) adopts technical grade product, and Tianjin Kermel Chemical Reagent Co., Ltd. produces.
Described 2-acrylamido-2-methyl propane sulfonic acid (AMPS) adopts technical grade product, and extra large chemical industry company limited produces in Juye County, Shandong Province.
Described initiator is an ammonium persulphate, is analytical pure, and Chemical Reagent Co., Ltd., Sinopharm Group produces.
Described chlorine bleach liquor is analytical pure (available chlorine content>10%), and Jin Bei Fine Chemical Co., Ltd in Tianjin produces.
Embodiment 2:
A kind of preparation method of amphoteric ion polymer fluid loss additive, it comprises the steps:
1) mass ratio by acrylamide (AM) and 2-acrylamido-2-methyl propane sulfonic acid (AMPS) is 5: 1, is dissolved in the water, and gets mixed solution A, and the mass concentration of mixed solution A is 20%;
2) mixed solution A is at 50 ℃, and pH value 7 adds under the initiator condition, and reaction 4h gets mixing solutions B, and wherein, initiator is 0.5% of acrylamide and 2-acrylamido-2-methyl propane sulfonic acid (AM and AMPS) quality;
3) mixing solutions B cools off with ice-water bath, treat temperature-stable after, by-CONH
2(amido): NaClO: NaOH=1: 0.5: 10 amount is reacted 8h than adding 1 ℃ the NaClO solution that contains NaOH in the ice-water bath, gets mixed solution C;
4) press HCl: NaOH=1 then: 1 amount must be glued the shape product than slowly adding HCl solution;
5) sticking shape product in methyl alcohol repeatedly agitator treating get the pale precipitation thing, take out throw out pelletizing, oven dry, pulverizing then and promptly get amphoteric ion polymer fluid loss additive product (yellow powder powder).
Described acrylamide (AM) adopts technical grade product, and Tianjin Kermel Chemical Reagent Co., Ltd. produces.
Described 2-acrylamido-2-methyl propane sulfonic acid (AMPS) adopts technical grade product, and extra large chemical industry company limited produces in Juye County, Shandong Province.
Described initiator is sodium bisulfite and ammonium persulphate, and the mass ratio of ammonium persulphate and sodium bisulfite is 2: 1, is analytical pure, and Chemical Reagent Co., Ltd., Sinopharm Group produces.
Described chlorine bleach liquor is analytical pure (available chlorine content>10%), and Jin Bei Fine Chemical Co., Ltd in Tianjin produces.
Embodiment 3:
A kind of preparation method of amphoteric ion polymer fluid loss additive, it comprises the steps:
1) mass ratio by acrylamide (AM) and 2-acrylamido-2-methyl propane sulfonic acid (AMPS) is 3: 1, is dissolved in the water, and gets mixed solution A, and the mass concentration of mixed solution A is 30%;
2) mixed solution A is at 70 ℃, and pH value 10 adds under the initiator condition, and reaction 6h gets mixing solutions B, and wherein, initiator is 1% of acrylamide and 2-acrylamido-2-methyl propane sulfonic acid (AM and AMPS) quality;
3) mixing solutions B cools off with ice-water bath, treat temperature-stable after, by-CONH
2(amido): NaClO: NaOH=1: 1: 10 amount is reacted 10h than adding 5 ℃ the NaClO solution that contains NaOH in the ice-water bath, gets mixed solution C;
4) press HCl: NaOH=1 then: 1 amount must be glued the shape product than slowly adding HCl solution;
5) sticking shape product in methyl alcohol repeatedly agitator treating get the pale precipitation thing, take out throw out pelletizing, oven dry, pulverizing then and promptly get amphoteric ion polymer fluid loss additive product (yellow powder powder).
Described acrylamide (AM) adopts technical grade product, and Tianjin Kermel Chemical Reagent Co., Ltd. produces.
Described 2-acrylamido-2-methyl propane sulfonic acid (AMPS) adopts technical grade product, and extra large chemical industry company limited produces in Juye County, Shandong Province.
Described initiator is sodium bisulfite and ammonium persulphate, and the mass ratio of ammonium persulphate and sodium bisulfite is 2: 1, is analytical pure, and Chemical Reagent Co., Ltd., Sinopharm Group produces.
Described chlorine bleach liquor is analytical pure (available chlorine content>10%), and Jin Bei Fine Chemical Co., Ltd in Tianjin produces.
Claims (2)
1. the preparation method of an amphoteric ion polymer fluid loss additive is characterized in that it comprises the steps:
1) mass ratio by acrylamide and 2-acrylamido-2-methyl propane sulfonic acid is 10: 1~3: 1, is dissolved in the water, and gets mixed solution A, and the mass concentration of mixed solution A is 8%~30%;
2) mixed solution A is at 35 ℃~70 ℃, and pH value 3~10 adds under the initiator condition, and reaction 3~6h gets mixing solutions B, and wherein, initiator is 0.1%~1% of acrylamide and 2-acrylamido-2-methyl propane sulfonic acid quality;
3) mixing solutions B cools off with ice-water bath, treat temperature-stable after, by-CONH
2: NaClO: NaOH=1: 0.1: 10~1: 1: 10 amount is reacted 5~10h than adding-10 ℃~5 ℃ the NaClO solution that contains NaOH in the ice-water bath, gets mixed solution C;
4) press HCl: NaOH=1 then: 1 amount must be glued the shape product than adding HCl solution;
5) sticking shape product agitator treating in methyl alcohol gets the pale precipitation thing, takes out throw out pelletizing, oven dry, pulverizing then and promptly gets the amphoteric ion polymer fluid loss additive product.
2. the preparation method of a kind of amphoteric ion polymer fluid loss additive according to claim 1, it is characterized in that: described initiator is an ammonium persulphate; Perhaps be ammonium persulphate and sodium bisulfite, the mass ratio of ammonium persulphate and sodium bisulfite is 2: 1.
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CN100595254C true CN100595254C (en) | 2010-03-24 |
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CN101619209B (en) * | 2009-07-31 | 2013-05-08 | 中国石油化工股份有限公司胜利油田分公司采油工艺研究院 | New application and composition of amide sodium sulfonate as oil field additive |
CN103881021B (en) * | 2014-03-17 | 2016-02-24 | 西南石油大学 | A kind of aluminate cement slurry system water retaining and preparation method thereof |
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Non-Patent Citations (4)
Title |
---|
AMPS共聚物固井降失水剂的合成及性能研究. 王展旭等.青岛科技大学学报,第25卷第4期. 2004 |
AMPS共聚物固井降失水剂的合成及性能研究. 王展旭等.青岛科技大学学报,第25卷第4期. 2004 * |
阴离子型AM/AMPS共聚物的合成及性能评价. 赵田红等.精细石油化工进展,第赵田红 等卷第7期. 2006 |
阴离子型AM/AMPS共聚物的合成及性能评价. 赵田红等.精细石油化工进展,第赵田红 等卷第7期. 2006 * |
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