JPS5915417A - Production of dispersant - Google Patents

Production of dispersant

Info

Publication number
JPS5915417A
JPS5915417A JP57125100A JP12510082A JPS5915417A JP S5915417 A JPS5915417 A JP S5915417A JP 57125100 A JP57125100 A JP 57125100A JP 12510082 A JP12510082 A JP 12510082A JP S5915417 A JPS5915417 A JP S5915417A
Authority
JP
Japan
Prior art keywords
water
polymerization
meth
solution
monomer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP57125100A
Other languages
Japanese (ja)
Other versions
JPH0253092B2 (en
Inventor
Hisao Takeda
久雄 武田
Katsutoshi Tanaka
勝利 田中
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Rei Technologies Inc
Kyoritsu Yuki Kogyo Kenkyusho KK
Original Assignee
Rei Technologies Inc
Kyoritsu Yuki Kogyo Kenkyusho KK
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Rei Technologies Inc, Kyoritsu Yuki Kogyo Kenkyusho KK filed Critical Rei Technologies Inc
Priority to JP57125100A priority Critical patent/JPS5915417A/en
Publication of JPS5915417A publication Critical patent/JPS5915417A/en
Publication of JPH0253092B2 publication Critical patent/JPH0253092B2/ja
Granted legal-status Critical Current

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  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Polymerisation Methods In General (AREA)

Abstract

PURPOSE:To produce a dry polymer solid suitable as an agent for dispersing bentonite in water, by adding an azo catalyst and a reducing agent to a specified aqueous solution of an acrylic monomer, and polymerizing it while evaporating the water by the heat of polymerization. CONSTITUTION:(Meth)acrylic acid is mixed with (meth)acrylamide at a molar ratio of 100:0-50:50, and an ammonia water, etc., are added to this mixture to form an aqueous monomer solution in which at least 60% of the (meth)acrylate acid has been converted into a salt and which contains 40-60wt%, based on (meth)acrylic acid, water.Then, to this aqueous monomer solution are added an azo catalyst (e.g., azobisisobutyronitrile) and an amount of a reducing agent (e.g., sodium hydrogensulfite) sufficient to reduce the total dissolved oxygen in the monomer, and the monomer solution is subjected to polymerization while the water is being evaporated by the heat of polymerization.

Description

【発明の詳細な説明】 本発明は安定液の製法に関するものであり。[Detailed description of the invention] The present invention relates to a method for producing a stabilizer.

詳しくは安定液に用いるぺ/トナイトの分散剤として使
用可能なポリマーの製法に関するものである。
Specifically, the present invention relates to a method for producing a polymer that can be used as a dispersant for Pe/tonite used in a stabilizing liquid.

安定液とはポーリング、連続壁工法等において土層掘削
時に掘削空間に充填し、内圧を高める事によシ土層壁の
崩壊を防止し、かつ混入する土砂を液中に保持する目的
で使用する液の総称である。
Stabilizing liquid is used to fill the excavated space during soil layer excavation in poling, continuous wall construction methods, etc., and prevent the collapse of the soil layer wall by increasing the internal pressure, and also to retain the soil and sand mixed in the liquid. It is a general term for liquids that

従来ベントナイトの分散剤として用いられてきたOMO
は天然物であシ、微生物により分解する結果腐敗によシ
急速に効果を失なう。
OMO has traditionally been used as a dispersant for bentonite.
Since it is a natural product, it rapidly loses its effectiveness due to putrefaction as a result of being decomposed by microorganisms.

腐敗した泥水にOMOを追加してもたちまち分解し効果
の回復は望めないため、腐敗した泥水は棄てるほかは無
かった。これを防止するには水溶性アクリルポリマーの
如き微生物分解をうけない合成物で安定液を調整する事
が望ましい。前述の様に安定液に用いる分散剤は液中に
土砂を保持するため増粘作用を持つ必要がある。
Even if OMO was added to the putrid muddy water, it would decompose immediately and the effect could not be restored, so there was no choice but to throw away the putrid muddy water. To prevent this, it is desirable to prepare the stabilizer with a synthetic material that is not subject to microbial decomposition, such as a water-soluble acrylic polymer. As mentioned above, the dispersant used in the stabilizing liquid needs to have a thickening effect in order to retain the earth and sand in the liquid.

しかし通常市販されている水溶性アクリルポリマーは液
中に混入した土砂を凝集させる性質があり分散剤として
使用できない。
However, commercially available water-soluble acrylic polymers cannot be used as dispersants because they have the property of agglomerating earth and sand mixed into the liquid.

又非常に低分子量のアクリルポリマーは凝集作用を示さ
ないが増粘作用を持たぬため安定a¥に用いる事ができ
ない。 。
Also, acrylic polymers with very low molecular weights do not exhibit a flocculating effect, but they do not have a thickening effect, so they cannot be used for stable a\. .

この様な従来の水溶性ポリマーの性質は重合条件による
ものであシレドツクス系あるいはア件 ゾ系触媒による重合物に共通の蛾質である。
The properties of such conventional water-soluble polymers depend on the polymerization conditions, and are common to polymers produced using redox-based or azo-based catalysts.

本発明者はかかる条件を種々検討の結果還元剤とアゾ系
触媒を併用して重合する事により。
The present inventor conducted a polymerization using a reducing agent and an azo catalyst together as a result of various studies on such conditions.

安定液に使用可能な増粘作用のある分散剤を製造し得る
事を発見し本発明に到達した。
We have discovered that it is possible to produce a dispersant with a thickening effect that can be used in stabilized liquids, and have arrived at the present invention.

本発明におけるポリマーが特異的に有効である理由は不
明であるが高分子の分子構造に起弧するものと考える。
Although the reason why the polymer in the present invention is specifically effective is unknown, it is thought to be due to the molecular structure of the polymer.

本発明に用いられる水溶性アクリルポリマーとしては(
メタ)アクリル酸と(メタ)アクリルアミドのモル比が
100:O〜50:50  の組成を持ちかつアクリル
酸は60%以上がアミン。
The water-soluble acrylic polymer used in the present invention is (
The composition has a molar ratio of meth)acrylic acid and (meth)acrylamide of 100:0 to 50:50, and 60% or more of the acrylic acid is amine.

アンモニウム、アルカリ金属によシ中和されアクリル酸
塩の形を取っている事が望ましい。
Preferably, it is in the form of an acrylate that has been neutralized with ammonium or an alkali metal.

重合開始の触媒としてはアゾビスイ:ノブチロ=l−!
J/L=、7ゾビスイソシアノ吉草酸、アゾヒスアミジ
ノプロパン等アゾ系触媒が適当であり過硫酸塩、過酸化
水素、有機過酸化物は不適である。還元剤としては亜硫
酸塩、亜硫酸水素塩が最も望ましい。亜二チオン酸塩、
チオ硫酸塩は性能が劣シ、硫酸第一鉄の如き重金属イオ
ンは効果が無い。
As a catalyst for polymerization initiation, azobisui:Nobutyro=l-!
J/L=, 7zobisisocyanovaleric acid, azo-based catalysts such as azohisamidinopropane are suitable, and persulfates, hydrogen peroxide, and organic peroxides are unsuitable. Sulfites and hydrogen sulfites are most preferred as reducing agents. dithionite,
Thiosulfates have poor performance, and heavy metal ions such as ferrous sulfate are ineffective.

これら還元剤はモノマー中の溶存酸素を全量消費する量
以上に加えられ1通常モノマー溶液に対し50〜50,
000ppmの範囲で所望の粘度となる様に選ばれる。
These reducing agents are added in an amount more than enough to consume the entire amount of dissolved oxygen in the monomer, and are usually added at a concentration of 50 to 50% per monomer solution.
The desired viscosity is selected within the range of 0,000 ppm.

重合時のモノマー溶液の濃度は重要でありアクリルモノ
マーに対し40〜60重量%の水分量に調整する事によ
り1重合熱により水分を気化せしめ重合後乾燥工程を経
る事無く粉砕し微細な粉末を得る事ができる。
The concentration of the monomer solution during polymerization is important, and by adjusting the water content to 40 to 60% by weight relative to the acrylic monomer, the water can be vaporized by the heat of one polymerization, and after polymerization, it can be pulverized into a fine powder without going through a drying process. You can get it.

得られた粉末に炭酸ソーダの如きアルカリ金属塩を混合
する事にょシ溶解性を向上させる事もできる。
The solubility can also be improved by mixing an alkali metal salt such as soda carbonate with the obtained powder.

水蒸気の輝散に便ならしむるため重合容器は上部が開放
している必要があシ、エンドレスベルト上で重合する事
が好結果を与える。
The polymerization vessel must be open at the top to allow the water vapor to diffuse away, and polymerization on an endless belt gives good results.

以下実施例により本発明を具体的に説明する。The present invention will be specifically explained below using Examples.

実施例1 アクリル酸72グに30% アン・モニア水351を3
0℃に冷却しながら混合してモノマー溶液を調整しAI
BNQ、7fをアセトン7meに溶解した液を混合後、
亜硫酸水素ナトリウム21をアンモニア水87に溶解し
た液を添加混合しただちにテフロンコーティング浅皿中
で重合を行ない乾燥減量9%のポリマー乾燥固体を得た
Example 1 30% ammonia water 351 to 72 g of acrylic acid
Mix while cooling to 0°C to prepare the monomer solution and add AI
After mixing a solution of BNQ, 7f dissolved in acetone 7me,
Immediately after adding and mixing 21 parts of sodium bisulfite dissolved in 87 parts of aqueous ammonia, polymerization was carried out in a Teflon-coated shallow dish to obtain a dry polymer solid having a drying loss of 9%.

粉砕後IN食塩水中にポリマー濃度】%に溶解゛1シ回
転回転計にて測定した25℃における粘度は8.5cp
であった。
After pulverization, the polymer concentration was dissolved in IN saline solution at a concentration of 1%.The viscosity at 25°C measured with a rotation meter was 8.5 cp.
Met.

本粉末を試料1とする。This powder is designated as Sample 1.

比較例1 アクリル酸72yに30% アンモニア水43グを30
℃に冷却しながら混合してモノマー溶液を調整し、AI
BNo、71i’  と ドデシルメルカプタン0.0
77をアセトン7mlに溶解した液を混合後ただちにテ
フロン浅皿中に移して重合させ乾燥減量9%。
Comparative Example 1 30% ammonia water 43g to 72y acrylic acid
Prepare the monomer solution by mixing while cooling to
BNo. 71i' and dodecyl mercaptan 0.0
Immediately after mixing, a solution of 77 dissolved in 7 ml of acetone was transferred to a Teflon shallow dish and polymerized, resulting in a drying loss of 9%.

INN食塩水中1溶溶液粘8.7cpのポリマー乾燥固
体を得た。
One solution in INN saline solution yielded a dry polymer solid with a viscosity of 8.7 cp.

本粉末を試料2とする。This powder is designated as Sample 2.

実施例2 アクリルアミド287.アクリル酸11グ、アクリル酸
カリウム501.水267の混合溶液にル アゾビスアミジノプロパン塩酸塩07’%、亜硫酸水素
ナトリウム7 tqを水41i’に溶解した液を添加混
合後ただちにテフロンコーティング浅皿に移して゛□重
合させ乾燥減量9.5%、INN食塩水中1溶溶液粘8
.5cpのポリマー乾燥固体を得た。
Example 2 Acrylamide 287. 11 grams of acrylic acid, 501 grams of potassium acrylate. A solution prepared by dissolving 07'% of ruazobisamidinopropane hydrochloride and 7 tq of sodium hydrogen sulfite in 41 i' of water was added to a mixed solution of 267 ml of water. After mixing, the solution was immediately transferred to a Teflon-coated shallow dish and allowed to polymerize, resulting in a drying loss of 9.5 ml. %, INN 1 solution viscosity in saline solution 8
.. 5 cp of polymer dry solid was obtained.

本粉末を試料3とする。This powder is designated as sample 3.

比較例2 亜硫酸水素ナトリウムを加えない事以外の条件は実施例
2と同一の条件で重合を行ない乾燥減量9.5%、IN
N食塩水中1溶溶液粘9.7Cpのポリマー乾燥固体を
得た。
Comparative Example 2 Polymerization was carried out under the same conditions as Example 2 except that sodium bisulfite was not added, and the loss on drying was 9.5%, IN
A solution of 1 in N saline solution yielded a dry polymer solid with a viscosity of 9.7 Cp.

本粉末を試料溢とする。Fill the sample with this powder.

効果試験 水道水700m6をミキサー中で撹拌しながらベントナ
イト42グを加え、3分後に分散剤2%水溶液10罰を
添加し、さらに5分間撹拌を続ける。
Effect test 42 g of bentonite is added to 700 m6 of tap water while stirring in a mixer, 3 minutes later, 10 g of a 2% aqueous dispersant solution is added, and stirring is continued for an additional 5 minutes.

−晩静置後スターラーで5分間撹拌をした後ファンネル
粘性とP水量を測定した。
- After standing still overnight, the mixture was stirred with a stirrer for 5 minutes, and the funnel viscosity and P water amount were measured.

ファンネル粘性の測定はファンネル粘度計(500rn
e/ 500 rrtl )の秒数、P水量はAPI規
格濾過試験機にて3’ kg / crrt・30分に
おけるm/数である。
Funnel viscosity can be measured using a funnel viscometer (500rn
e/500 rrtl) in seconds, and the P water amount is m/number in 3' kg/crrt/30 minutes using an API standard filtration tester.

Claims (1)

【特許請求の範囲】[Claims] アクリル酸とアクリルアミドのモル比が100二〇〜5
0:50であシ、かつアクリル酸の60%以上がアクリ
ル酸塩の形を取シ、全アクリルモノマーに対し水分量が
40〜60重量%である七ツマー水溶液に、アゾ系触媒
を添加して重合させ1重合熱によ多水分を蒸発させて乾
燥固体を得るにあたり、モノマー溶液に対し50〜50
000ppmの還元剤を添加する事を特長とする安定液
調整用分散剤の製造方法。
The molar ratio of acrylic acid and acrylamide is 10020 to 5
An azo catalyst is added to a seven-mer aqueous solution in which the ratio is 0:50, 60% or more of the acrylic acid is in the form of acrylate, and the water content is 40 to 60% by weight based on the total acrylic monomer. 50 to 50
A method for producing a dispersant for adjusting a stable liquid, characterized by adding 000 ppm of a reducing agent.
JP57125100A 1982-07-20 1982-07-20 Production of dispersant Granted JPS5915417A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP57125100A JPS5915417A (en) 1982-07-20 1982-07-20 Production of dispersant

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP57125100A JPS5915417A (en) 1982-07-20 1982-07-20 Production of dispersant

Publications (2)

Publication Number Publication Date
JPS5915417A true JPS5915417A (en) 1984-01-26
JPH0253092B2 JPH0253092B2 (en) 1990-11-15

Family

ID=14901849

Family Applications (1)

Application Number Title Priority Date Filing Date
JP57125100A Granted JPS5915417A (en) 1982-07-20 1982-07-20 Production of dispersant

Country Status (1)

Country Link
JP (1) JPS5915417A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5213893A (en) * 1990-09-14 1993-05-25 Nippon Shokubai Co., Ltd. Waterproofing agent for cable

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57125098A (en) * 1980-12-16 1982-08-04 Burroughs Corp Mail letter

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57125098A (en) * 1980-12-16 1982-08-04 Burroughs Corp Mail letter

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5213893A (en) * 1990-09-14 1993-05-25 Nippon Shokubai Co., Ltd. Waterproofing agent for cable

Also Published As

Publication number Publication date
JPH0253092B2 (en) 1990-11-15

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