CN104140453A - Preparation method of glyceryl glucoside for drilling fluid - Google Patents
Preparation method of glyceryl glucoside for drilling fluid Download PDFInfo
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- CN104140453A CN104140453A CN201310524571.0A CN201310524571A CN104140453A CN 104140453 A CN104140453 A CN 104140453A CN 201310524571 A CN201310524571 A CN 201310524571A CN 104140453 A CN104140453 A CN 104140453A
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Abstract
Belonging to technical field of oilfield chemical drilling fluid treatment agents, the invention discloses a preparation method of glyceryl glucoside for drilling fluid. The method includes the steps of: (1) adding glucose and glycerin into a reaction bottle in a mole ratio of 1:4-8, adding a protonic acid loaded load type catalyst accounting for 20%-50% of the mass of glucose, carrying out stirring reaction at 80-120DEG C for 5-10h, and filtering out the load type catalyst to obtain an untreated glyceryl glucoside reaction solution; (2) lowering the temperature of the glyceryl glucoside reaction solution to 40-50DEG C, adjusting the pH value to 8.0-10.0 by a neutralizing agent, performing filtering when the solution is hot, and separating out unreacted glucose, thus obtaining the glucose removed filtrate; and (3) transferring the glucose removed filtrate into a single-port flask, and conducting pressure reduced distillation to remove excess glycerin, thus obtaining a glyceryl glucoside crude product.
Description
Technical field
The present invention relates to the preparation method of a kind of drilling fluid glucoside derivative, particularly relate to the preparation method of a kind of drilling fluid glyceryl glucoside, belong to oilfield chemistry additive for drilling fluid technical field.
Background technology
Polylol glucoside is a kind of common compounds, can be used as humectant, wetting Agent for Printing Inks, emulsifying agent and tensio-active agent etc.Since the 1980's, make tensio-active agent resource and product design become the pressing problem being reconsidered to the concern of environment, developing natural reproducible resource production tensio-active agent is one of main method of dealing with problems.From world wide, starch is cheap, the abundantest natural reproducible resource, and glucose is the chain link of starch, and its reactive behavior and reaction preference make it become the key substance of the multi-functional derivative of preparation.Utilize starch and hydrolysate derivative thereof can produce polylol glucoside.China is large agricultural country, and starch resource is very abundant, and this series products prepare simple, exploitation polylol glucoside also there is certain feasibility and necessity.
Common polylol glucoside has ethylene glycol glucoside, propylene glycol glucoside, diethyleneglycol glucoside, glycosylglycerol etc.Conventional preparation method of the prior art as: directly glycosidation method, solvent method, turn glucosides method, indirect synthesis technique or enzyme catalysis method etc.
Directly glycosidation method is by first glucose acetobrom, makes acetobrom glucose crystal, then joins in ethylene glycol, and adds dry Ag
2cO
3vibration, then place after adding dry-out benzene vibration, remove Ag salt, mixture separation.With dry-out benzene re-extract ethylene glycol layer, extraction liquid obtains mono-glucoside four acetate of ethylene glycol B-D-through condensing crystal, then takes off vinegar acidification reaction by Fischer method, finally obtains the mono-glucoside crystal of ethylene glycol B-D-.The method preparation process is loaded down with trivial details, industrial difficult realization.
Starch and polyvalent alcohol directly carry out glycosyl shift reaction can synthetic starch polyol.Nineteen sixty is for mid-term, and the U.S. utilizes starch and ethylene glycol to carry out Transglycosylation to have synthesized this polyol the earliest.In generation nineteen ninety, Jin Zhengyu has studied the Transglycosylation of starch and polyvalent alcohol at home, this reaction have transform easily, cost is low, theoretical yield advantages of higher.But the polyhydroxylated starch quality preparing taking starch as raw material is poor, and by product is more, uses glucose and polyol reaction instead and can obtain the good polylol glucoside product of quality.
Summary of the invention
The object of the invention is the more shortcoming of product by product obtaining in order to overcome existing polyvalent alcohol glucosides technology of preparing, provide a kind of reaction times shorter, catalyzer is recyclable, the drilling fluid that production cost the is lower preparation method of glyceryl glucoside.
Concrete steps are as follows:
(1) glucose and glycerine are added to reaction flask for 1:4～8 in molar ratio, the loaded catalyst of load protonic acid adds by 20%～50% of glucose quality, stirring reaction 5～10h at 80～120 DEG C of temperature, filter out loaded catalyst, obtain untreated glyceryl glucoside reaction solution;
(2) glyceryl glucoside reacting liquid temperature is down to 40～50 DEG C, with neutralizing agent adjusting pH value to 8.0～10.0, filtered while hot, isolates unreacted glucose, obtains removing the filtrate of glucose;
(3) filtrate that removes glucose is moved into single port flask, excessive glycerine is removed in underpressure distillation, obtains the thick product of glyceryl glucoside.
Described neutralizing agent is the one in sodium hydroxide, potassium hydroxide, sodium carbonate.
The concrete preparation process of described loaded catalyst is as follows:
(1) be that 4～10 object gacs activate 6～10h under 300～500 DEG C of high temperature by particle diameter, preparing specific surface area is 700～1500m
2the supported catalyst agent carrier of/g;
(2) protonic acid being made into mass concentration is 10%～30% the aqueous solution, as the steeping fluid of support of the catalyst;
(3) supported catalyst agent carrier is mixed for 1:2～4 in mass ratio with the steeping fluid of support of the catalyst, dipping 24～48h, obtains the catalyzer after dipping;
(4) the catalyzer suction filtration after dipping is removed to filtrate, the loaded catalyst of not dried, by the loaded catalyst of not drying dry 4～8h at 100～110 DEG C, makes loaded catalyst.
Described gac is the one in cocoanut active charcoal, wood activated charcoal, coal mass active carbon;
Described protonic acid is mineral acid, organic acid or mineral acid and the composite mixture of organic acid;
Described mineral acid is the one in sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, phospho-wolframic acid;
Described organic acid is the one in tosic acid, Witco 1298 Soft Acid, thionamic acid.
The invention has the beneficial effects as follows:
It is that raw material is prepared glyceryl glucoside under the condition of loaded catalyst catalysis that the present invention adopts glucose and glycerine, because in reaction process with loaded catalyst catalysis, reaction times is shorter, the recyclable recycling of catalyzer, production cost is lower, product application, in drilling fluid, can be played good restraining effect and lubrication.
Embodiment
Loaded catalyst Preparation Example 1
Cocoanut active charcoal is activated to 6h under 300 DEG C of high temperature, obtain supported catalyst agent carrier; It is 10% the aqueous solution that tosic acid is made into mass concentration, prepares the steeping fluid of support of the catalyst; By supported catalyst agent carrier with the steeping fluid of support of the catalyst in mass ratio for 1:2 mixes, dipping 24h, obtain dipping after catalyzer; Catalyzer suction filtration after dipping is removed to filtrate, the loaded catalyst of not dried, at 100 DEG C, dry 4h, makes the loaded catalyst A for preparing alkyl glycoside.
Embodiment 2～10 steps are identical with embodiment 1, and concrete raw materials consumption and the preparation condition table of loaded catalyst are as shown in table 1:
Table 1 loaded catalyst raw materials consumption and preparation condition table
Glyceryl glucoside Preparation Example 1
In the 500mL four-hole boiling flask that thermometer, prolong, water trap are housed, add the loaded catalyst A18g of glucose 90g, glycerine 184g and load tosic acid, at normal pressure, at 80 DEG C of temperature, react 5h, obtain faint yellow transparent glyceryl glucoside reaction solution; Filtrate temperature is down to 90 DEG C, and the sodium hydroxide solution with 30% regulates pH value to 8.0, and filtered while hot, isolates unreacted glucose, obtains removing the filtrate of glucose; The filtrate that removes glucose is moved into single port flask, and excessive glycerine is removed in underpressure distillation, obtains the thick product of glyceryl glucoside, and glyceryl glucoside yield is 95.6%.1% product water solution extreme boundary lubrication coefficient is 0.06, and shale rolling primary recovery is 95.45%, and relative recovery is 99.31%.
Embodiment 2～10 steps are identical with embodiment 1, and concrete reactive material and reaction conditions are as shown in table 2:
Table 2 reactive material consumption, reaction conditions and product performance table
As shown in Table 1, it is that raw material is prepared glyceryl glucoside under the condition of loaded catalyst catalysis that the present invention adopts glucose and glycerine, and the present invention compared with prior art, reaction times is shorter, product yield is higher, the recyclable recycling of catalyzer, and production cost is lower.Product application, in drilling fluid, can be played good restraining effect and lubrication.As shown in Table 2,1% product water solution extreme boundary lubrication coefficient < 0.10, shale rolling primary recovery > 90%, relative recovery > 98%.
Claims (7)
1. a preparation method for glyceryl glucoside for drilling fluid, is characterized in that comprising the following steps:
(1) glucose and glycerine are added to reaction flask for 1:4～8 in molar ratio, the loaded catalyst of load protonic acid adds by 20%～50% of glucose quality, stirring reaction 5～10h at 80～120 DEG C of temperature, filter out loaded catalyst, obtain untreated glyceryl glucoside reaction solution;
(2) glyceryl glucoside reacting liquid temperature is down to 40～50 DEG C, with neutralizing agent adjusting pH value to 8.0～10.0, filtered while hot, isolates unreacted glucose, obtains removing the filtrate of glucose;
(3) filtrate that removes glucose is moved into single port flask, excessive glycerine is removed in underpressure distillation, obtains the thick product of glyceryl glucoside.
2. the preparation method of glyceryl glucoside for drilling fluid as claimed in claim 1, is characterized in that described neutralizing agent is the one in sodium hydroxide, potassium hydroxide, sodium carbonate.
3. the preparation method of glyceryl glucoside for drilling fluid as claimed in claim 1, is characterized in that the described concrete preparation process of loaded catalyst is as follows:
(1) be that 4～10 object gacs activate 6～10h under 300～500 DEG C of high temperature by particle diameter, preparing specific surface area is 700～1500m
2the supported catalyst agent carrier of/g;
(2) protonic acid being made into mass concentration is 10%～30% the aqueous solution, as the steeping fluid of support of the catalyst;
(3) supported catalyst agent carrier is mixed for 1:2～4 in mass ratio with the steeping fluid of support of the catalyst, dipping 24～48h, obtains the catalyzer after dipping;
(4) the catalyzer suction filtration after dipping is removed to filtrate, the loaded catalyst of not dried, by the loaded catalyst of not drying dry 4～8h at 100～110 DEG C, makes loaded catalyst.
4. the preparation method of glyceryl glucoside for drilling fluid as claimed in claim 1, is characterized in that described gac is the one in cocoanut active charcoal, wood activated charcoal, coal mass active carbon.
5. the preparation method of glyceryl glucoside for drilling fluid as claimed in claim 1, is characterized in that described protonic acid is mineral acid, organic acid or mineral acid and the composite mixture of organic acid.
6. the preparation method of glyceryl glucoside for drilling fluid as claimed in claim 1, is characterized in that described mineral acid is the one in sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, phospho-wolframic acid.
7. the preparation method of glyceryl glucoside for drilling fluid as claimed in claim 1, is characterized in that described organic acid is the one in tosic acid, Witco 1298 Soft Acid, thionamic acid.
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| CN201310524571.0A CN104140453B (en) | 2013-10-29 | 2013-10-29 | A kind of preparation method of drilling fluid glyceryl glucoside |
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| CN201310524571.0A CN104140453B (en) | 2013-10-29 | 2013-10-29 | A kind of preparation method of drilling fluid glyceryl glucoside |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109694700A (en) * | 2017-10-23 | 2019-04-30 | 中石化石油工程技术服务有限公司 | A kind of water-base drilling fluid |
| CN110684060A (en) * | 2019-09-11 | 2020-01-14 | 上海吉奉生物科技有限公司 | Preparation method of alkyl glycoside by using sulfonated graphene catalyst |
| CN111423477A (en) * | 2020-05-28 | 2020-07-17 | 福建莲珂科技有限公司 | Polyol glucoside and preparation method and application thereof |
| CN115005488A (en) * | 2022-06-24 | 2022-09-06 | 湖北中烟工业有限责任公司 | Atomizing agent for cigarettes and electronic cigarette liquid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109694700A (en) * | 2017-10-23 | 2019-04-30 | 中石化石油工程技术服务有限公司 | A kind of water-base drilling fluid |
| CN110684060A (en) * | 2019-09-11 | 2020-01-14 | 上海吉奉生物科技有限公司 | Preparation method of alkyl glycoside by using sulfonated graphene catalyst |
| CN111423477A (en) * | 2020-05-28 | 2020-07-17 | 福建莲珂科技有限公司 | Polyol glucoside and preparation method and application thereof |
| CN115005488A (en) * | 2022-06-24 | 2022-09-06 | 湖北中烟工业有限责任公司 | Atomizing agent for cigarettes and electronic cigarette liquid |
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Effective date of registration: 20180723 Address after: 100029 Chaoyangmen North Street, Chaoyang District, Chaoyang District, Beijing Co-patentee after: Drilling Research Institute of Zhongyuan Petroleum Engineering Co., Ltd. Sinopec Patentee after: Sinopec Corp. Co-patentee after: SINOPEC OILFIELD SERVICE CORPORATION Co-patentee after: SINOPEC ZHONGYUAN PETROLEUM ENGINEERING CO., LTD. Address before: 100728 Chaoyangmen North Street, Chaoyang District, Chaoyang District, Beijing Co-patentee before: Drilling Research Institute of Zhongyuan Petroleum Engineering Co., Ltd. Sinopec Patentee before: Sinopec Corp. |