CN106045946A - Preparation method of sorbitan tristearate - Google Patents

Preparation method of sorbitan tristearate Download PDF

Info

Publication number
CN106045946A
CN106045946A CN201610480660.3A CN201610480660A CN106045946A CN 106045946 A CN106045946 A CN 106045946A CN 201610480660 A CN201610480660 A CN 201610480660A CN 106045946 A CN106045946 A CN 106045946A
Authority
CN
China
Prior art keywords
preparation
arlacel
mixture
acid
sorbitol
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
CN201610480660.3A
Other languages
Chinese (zh)
Other versions
CN106045946B (en
Inventor
王菲
王加国
王日成
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.)
JIANGSU HAI'AN PETROCHEMICAL PLANT
Original Assignee
JIANGSU HAI'AN PETROCHEMICAL PLANT
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 JIANGSU HAI'AN PETROCHEMICAL PLANT filed Critical JIANGSU HAI'AN PETROCHEMICAL PLANT
Priority to CN201610480660.3A priority Critical patent/CN106045946B/en
Publication of CN106045946A publication Critical patent/CN106045946A/en
Application granted granted Critical
Publication of CN106045946B publication Critical patent/CN106045946B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D307/00Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/02Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
    • C07D307/04Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members
    • C07D307/18Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D307/20Oxygen atoms

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

Abstract

The invention discloses a preparation method of sorbitan tristearate. The sorbitan tristearate comprises sorbitol, stearic acid and an acidic catalyst. The preparation method comprises the following steps: (1) putting the sorbitol, stearic acid and acidic catalyst in a reaction kettle, heating to 180-230 DEG C, and reacting for 4-8h to obtain a mixture A; (2) measuring the acid value of the mixture A, when the acid value of the mixture A is not greater than 10mgKOH/g, cooling to obtain the sorbitan tristearate, and when the acid value of the mixture A is greater than 10mgKOH/g, executing the step (3); and (3) putting the mixture A in the reaction kettle for reacting for 0.25-1h, and then executing the step (2). The preparation method of the sorbitan tristearate, provided by the invention, realizes one-step preparation of the sorbitan tristearate without colloid generation, thereby improving the quality of the sorbitan tristearate.

Description

The preparation method of Arlacel-65
Technical field
The disclosure relates generally to nonionic surfactant technical field, is specifically related to emulsifying agent, particularly relates to dehydration The preparation method of sorbitol tristearate.
Background technology
Surfactant is a kind of organic compound with special construction and character, and it is alternate that they can change two significantly Interfacial tension or the surface tension of liquid (generally water), there is the performances such as moistening foaming emulsifying washing.Surfactant Due to have moistening or anti-stick, emulsifying or breakdown of emulsion, foaming or froth breaking and solubilising, disperse, wash, anticorrosion, antistatic etc. are Row physics chemical action and corresponding actual application, become class fine chemical product versatile and flexible, broad-spectrum.Live in surface Property agent is except in daily life as detergent, other application almost can cover all of field of fine chemical.Live in surface Property agent is divided into ionic surfactant (including cationic surfactant and anion surfactant), non-ionic surface Activating agent, amphoteric surfactant, compound surfactant, other surfactants etc..Wherein, nonionic is as at aqueous solution In do not produce the surfactant of ion, the solubility with temperature in water raises and reduces.Nonionic surfactant has The diversities such as good washing, dispersion, emulsifying, foaming, moistening, solubilising, antistatic, level dyeing, anticorrosion, sterilization and protecting colloid Can, use extensively, good market prospect.
Arlacel-65 (in the art be frequently referred to S-65) as the representative of nonionic surfactant, It has functions such as being dispersed among petroleum ether, mineral oil, vegetable oil, be widely deployed medicine, cosmetics, weave, paint, Explosive Industry emulsifying agent, also can make textile oil preparation, make emulsifying agent in oil deep-well weighted mud, and dispersant is made in paint industry, Oil product is used as cosolvent and antirust agent.In the existing technique preparing Arlacel-65, generally adopt By the method for multi-step, particularly as follows: the first step, sorbitol is first reacted with catalyst for etherification;Second step, adds stearic acid and ester Change catalyst to react, finally obtain Arlacel-65.But above-mentioned preparation technology is loaded down with trivial details, needs staff To its monitored for prolonged periods of time, find that the reaction in the first step terminates, and then carries out second step operation in time, obtain anhydro sorbitol three stearic Acid esters.In preparation process, owing to sorbitol there will be intermolecular etherificate in etherification procedure, thus form the mistake of macromole Water sorbitol, i.e. colloid, there is impact to the use of Arlacel-65, such as, cause containing anhydrosorbitol in colloid The oil product that alcohol tristearate is made colloid when burning is easily formed waste residue, causes the appearance of the situation such as wear and tear in machines and blocking.
Summary of the invention
In view of drawbacks described above of the prior art or deficiency, it is desirable to provide an a kind of step preparation and the dehydration occurred without colloid The preparation method of sorbitol tristearate.
The present invention provides the preparation method of a kind of Arlacel-65, it is characterised in that anhydro sorbitol three Stearate includes sorbitol, stearic acid and acidic catalyst, and preparation method comprises the steps:
Step one: sorbitol, stearic acid are put in reactor with acidic catalyst, is warming up to 180~230 DEG C, during reaction Between be 4-8h, obtain mixture A;
Step 2: carry out mixture A surveying acid number, when the acid number of mixture A is not more than 10mgKOH/g, cooling, to obtain final product Arlacel-65;When the acid number of mixture A is more than 10mgKOH/g, go to step 3;
Step 3: continue to be placed in reaction kettle for reaction by mixture A, the response time is 0.25-1h, goes to step 2.
The preparation method of the Arlacel-65 that the present invention provides, by adding in sorbitol, stearic acid Acidic catalyst, and sorbitol, stearic acid are put in reactor together with acidic catalyst react, obtain anhydro sorbitol three Stearate, thus realize one-step method and prepare Arlacel-65.Additionally, also avoid the intermolecular ether of sorbitol Changing, thus realize producing without colloid, tool has an unexpected effect, and improves the quality of Arlacel-65.
Accompanying drawing explanation
By the detailed description that non-limiting example is made made with reference to the following drawings of reading, other of the application Feature, purpose and advantage will become more apparent upon:
The Arlacel-65 preparation method flow chart that Fig. 1 provides for the present invention.
Detailed description of the invention
With embodiment, the application is described in further detail below in conjunction with the accompanying drawings.It is understood that this place is retouched The specific embodiment stated is used only for explaining related invention, rather than the restriction to this invention.It also should be noted that, in order to It is easy to describe, accompanying drawing illustrate only and invent relevant part.
It should be noted that in the case of not conflicting, the embodiment in the application and the feature in embodiment can phases Combination mutually.Describe the application below with reference to the accompanying drawings and in conjunction with the embodiments in detail.
Embodiment 1
Refer to Fig. 1, the present embodiment provides the preparation method of a kind of Arlacel-65, anhydro sorbitol three Stearate includes sorbitol, stearic acid and acidic catalyst, and preparation method comprises the steps:
Step one: put in reactor by sorbitol, stearic acid and acidic catalyst, be warming up to 180 DEG C, the response time is 4h, obtains mixture A;
Step 2: carry out mixture A surveying acid number, when the acid number of mixture A is not more than 10mgKOH/g, cooling, to obtain final product Arlacel-65;When the acid number of mixture A is more than 10mgKOH/g, go to step 3;
Step 3: continue to be placed in reaction kettle for reaction by mixture A, the response time is 0.25-1h, goes to step 2.
Wherein, sorbitol and stearic molal weight are than 1:2, and acidic catalyst is sorbitol and stearic acid weight sum 0.2%, acidic catalyst is concentrated sulphuric acid and the pyrovinic acid of 98% concentration.
It addition, in the present embodiment after sorbitol, stearic acid react with acidic catalyst, the mixture A formed is surveyed Acid number, when the acid number of mixture A is more than 10mgKOH/g, continues to react in a kettle., after the question response time is 0.25-1h, Carry out again surveying acid number, during until the acid number of mixture A is not more than 10mgKOH/g, cooling, obtain anhydro sorbitol three stearic acid Ester.Here the question response time is preferably 0.25-1h, and the concrete time can be adjusted according to producing practical situation.
The Arlacel-65 that the present embodiment is prepared is yellow waxy solid, and hydroxyl value is 60KOH/g, soap Change value is 170mgKOH/g, and does not has colloid to occur.
Embodiment 2
Refer to Fig. 1, the present embodiment provides the preparation method of a kind of Arlacel-65, anhydro sorbitol three Stearate includes sorbitol, stearic acid and acidic catalyst, and preparation method comprises the steps:
Step one: put in reactor by sorbitol, stearic acid and acidic catalyst, be warming up to 190 DEG C, the response time is 8h, obtains mixture A;
Step 2: carry out mixture A surveying acid number, when the acid number of mixture A is not more than 10mgKOH/g, cooling, to obtain final product Arlacel-65;When the acid number of mixture A is more than 10mgKOH/g, go to step 3;
Step 3: continue to be placed in reaction kettle for reaction by mixture A, the response time is 0.25-1h, goes to step 2.
Wherein, sorbitol and stearic molal weight than 1:2.5, acidic catalyst be sorbitol and stearic acid weight it The 0.4% of sum, acidic catalyst is the concentrated sulphuric acid of 98% concentration, phosphorous acid, hypophosphorous acid and pyrovinic acid, and the weight ratio of four Example is 1:3:3:2.
It addition, in the present embodiment after sorbitol, stearic acid react with acidic catalyst, the mixture A formed is surveyed Acid number, when the acid number of mixture A is more than 10mgKOH/g, continues to react in a kettle., after the question response time is 0.25-1h, Carry out again surveying acid number, during until the acid number of mixture A is not more than 10mgKOH/g, cooling, obtain anhydro sorbitol three stearic acid Ester.Here the question response time is preferably 0.25-1h, and the concrete time can be adjusted according to producing practical situation.
The Arlacel-65 that the present embodiment is prepared is yellow waxy solid, and hydroxyl value is 68KOH/g, soap Change value is 181mgKOH/g, and does not has colloid to occur.
Embodiment 3
Refer to Fig. 1, the present embodiment provides the preparation method of a kind of Arlacel-65, anhydro sorbitol three Stearate includes sorbitol, stearic acid and acidic catalyst, and preparation method comprises the steps:
Step one: put in reactor by sorbitol, stearic acid and acidic catalyst, be warming up to 210 DEG C, the response time is 7h, obtains mixture A;
Step 2: carry out mixture A surveying acid number, when the acid number of mixture A is not more than 10mgKOH/g, cooling, to obtain final product Arlacel-65;When the acid number of mixture A is more than 10mgKOH/g, go to step 3;
Step 3: continue to be placed in reaction kettle for reaction by mixture A, the response time is 0.25-1h, goes to step 2.
Wherein, sorbitol and stearic molal weight than 1:2.5, acidic catalyst be sorbitol and stearic acid weight it The 0.6% of sum, acidic catalyst is phosphorous acid, hypophosphorous acid and pyrovinic acid, and the part by weight of three is 1:2:1.
It addition, in the present embodiment after sorbitol, stearic acid react with acidic catalyst, the mixture A formed is surveyed Acid number, when the acid number of mixture A is more than 10mgKOH/g, continues to react in a kettle., after the question response time is 0.25-1h, Carry out again surveying acid number, during until the acid number of mixture A is not more than 10mgKOH/g, cooling, obtain anhydro sorbitol three stearic acid Ester.Here the question response time is preferably 0.25-1h, and the concrete time can be adjusted according to producing practical situation.
The Arlacel-65 that the present embodiment is prepared is yellow waxy solid, and hydroxyl value is 80KOH/g, soap Change value is 185mgKOH/g, and does not has colloid to occur.
Embodiment 4
Refer to Fig. 1, the present embodiment provides the preparation method of a kind of Arlacel-65, anhydro sorbitol three Stearate includes sorbitol, stearic acid and acidic catalyst, and preparation method comprises the steps:
Step one: put in reactor by sorbitol, stearic acid and acidic catalyst, be warming up to 230 DEG C, the response time is 7h, obtains mixture A;
Step 2: carry out mixture A surveying acid number, when the acid number of mixture A is not more than 10mgKOH/g, cooling, to obtain final product Arlacel-65;When the acid number of mixture A is more than 10mgKOH/g, go to step 3;
Step 3: continue to be placed in reaction kettle for reaction by mixture A, the response time is 0.25-1h, goes to step 2.
Wherein, sorbitol and stearic molal weight are than 1:3, and acidic catalyst is sorbitol and stearic acid weight sum 0.6%, acidic catalyst is phosphoric acid, phosphorous acid and hypophosphorous acid, and the part by weight of three is 2:4:1.
It addition, in the present embodiment after sorbitol, stearic acid react with acidic catalyst, the mixture A formed is surveyed Acid number, when the acid number of mixture A is more than 10mgKOH/g, continues to react in a kettle., after the question response time is 0.25-1h, Carry out again surveying acid number, during until the acid number of mixture A is not more than 10mgKOH/g, cooling, obtain anhydro sorbitol three stearic acid Ester.Here the question response time is preferably 0.25-1h, and the concrete time can be adjusted according to producing practical situation.
The Arlacel-65 that above-described embodiment 1-4 prepares is all in yellow waxy solid, and hydroxyl value is 60 ~80KOH/g, saponification number are 170~190mgKOH/g, and colloid is not had to occur.
In sum, in above-described embodiment 1-4, by adding acidic catalyst in sorbitol, stearic acid, and by mountain Pears alcohol, stearic acid are put in reactor together with acidic catalyst and are reacted, thus realize one-step method and prepare anhydro sorbitol three Stearate.Additionally, also avoid the intermolecular etherificate of sorbitol, thus realize producing without colloid, there is beyond thought effect Really, improve the quality of Arlacel-65.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.People in the art Member should be appreciated that invention scope involved in the application, however it is not limited to the technology of the particular combination of above-mentioned technical characteristic Scheme, also should contain in the case of without departing from described inventive concept simultaneously, above-mentioned technical characteristic or its equivalent feature carry out Combination in any and other technical scheme of being formed.Such as features described above has similar merit with (but not limited to) disclosed herein The technical scheme that the technical characteristic of energy is replaced mutually and formed.

Claims (7)

1. the preparation method of an Arlacel-65, it is characterised in that described Arlacel-65 Including sorbitol, stearic acid and acidic catalyst, described preparation method comprises the steps:
Step one: described sorbitol, described stearic acid are put in reactor with described acidic catalyst, is warming up to 180~230 DEG C, the response time is 4-8h, obtains mixture A;
Step 2: carry out described mixture A surveying acid number, when the acid number of described mixture A is not more than 10mgKOH/g, cooling, Obtain described Arlacel-65;When the acid number of described mixture A is more than 10mgKOH/g, go to step 3;
Step 3: continue to be placed in reaction kettle for reaction by mixture A, the response time is 0.25-1h, goes to step 2.
The preparation method of Arlacel-65 the most according to claim 1, it is characterised in that described sorbitol With described stearic molal weight than 1:(2~3), described acidic catalyst be described sorbitol and described stearic acid weight it The 0.2%~0.8% of sum.
The preparation method of Arlacel-65 the most according to claim 1, it is characterised in that described dehydration mountain Pears alcohol tristearate is yellow waxy solid.
The preparation method of Arlacel-65 the most according to claim 1, it is characterised in that described dehydration mountain The hydroxyl value of pears alcohol tristearate is 60~80mgKOH/g.
The preparation method of Arlacel-65 the most according to claim 1, it is characterised in that described dehydration mountain The saponification number of pears alcohol tristearate is 170~190mgKOH/g.
The preparation method of Arlacel-65 the most according to claim 1, it is characterised in that described step one In temperature be 210 DEG C.
The preparation method of Arlacel-65 the most according to claim 1, it is characterised in that described acidity is urged Agent includes in the concentrated sulphuric acid of 98% concentration, pyrovinic acid, phosphoric acid, phosphorous acid, hypophosphorous acid in one or several mixing.
CN201610480660.3A 2016-06-28 2016-06-28 The preparation method of Arlacel-65 Expired - Fee Related CN106045946B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610480660.3A CN106045946B (en) 2016-06-28 2016-06-28 The preparation method of Arlacel-65

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610480660.3A CN106045946B (en) 2016-06-28 2016-06-28 The preparation method of Arlacel-65

Publications (2)

Publication Number Publication Date
CN106045946A true CN106045946A (en) 2016-10-26
CN106045946B CN106045946B (en) 2018-08-14

Family

ID=57166549

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610480660.3A Expired - Fee Related CN106045946B (en) 2016-06-28 2016-06-28 The preparation method of Arlacel-65

Country Status (1)

Country Link
CN (1) CN106045946B (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1228774A (en) * 1996-07-31 1999-09-15 帝国化学工业公司 Process for producing fatty acid esters of sorbitan as surfactants
CN1274351A (en) * 1997-10-07 2000-11-22 亨凯尔公司 Process for removing polysorbitols from sorbitan esters
CN103087015A (en) * 2012-12-19 2013-05-08 湖北葛店人福药用辅料有限责任公司 Preparation method of sorbitan oleate servicing as medicinal auxiliary material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1228774A (en) * 1996-07-31 1999-09-15 帝国化学工业公司 Process for producing fatty acid esters of sorbitan as surfactants
CN1274351A (en) * 1997-10-07 2000-11-22 亨凯尔公司 Process for removing polysorbitols from sorbitan esters
CN103087015A (en) * 2012-12-19 2013-05-08 湖北葛店人福药用辅料有限责任公司 Preparation method of sorbitan oleate servicing as medicinal auxiliary material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
毛连山等: "优质失水山梨醇单硬脂酸醋的合成", 《化学工业与工程技术》 *

Also Published As

Publication number Publication date
CN106045946B (en) 2018-08-14

Similar Documents

Publication Publication Date Title
CN104120624B (en) Emulsion type defoaming agent of biodiesel base and preparation method thereof
Rosen et al. Surfactants and interfacial phenomena
CN107236530B (en) A kind of water-base viscosity-reducing agent of emulsified superthick oil and preparation method thereof
Porter Handbook of surfactants
CN103980869B (en) A kind of oil base drilling fluid solid emulsifier and preparation method and the application in oil base drilling fluid
US2965678A (en) Polyoxyethylene ethers of branched chain alcohols
GB719445A (en) Branched chain alcohol derivatives
CN103387486B (en) A kind of preparation method of isomeric alcohol polyoxypropylene polyoxyethylene ether
US2923724A (en) Process of preparing ester type anionic surface active agents
WO2017023665A1 (en) Mixed dimers from alpha-olefin sulfonic acids
US2679462A (en) Strip-resistant bituminous composition
Bhatkhande et al. Ultrasound assisted PTC catalyzed saponification of vegetable oils using aqueous alkali
CN102336901A (en) Method for preparing polyurethane polyether polyol by waste oil
Abraham et al. The Influence of Surfactant Concentration and Surfactant Type on the Interfacial Tension of Heavy Crude Oil/Brine/Surfactant System.
US11168284B2 (en) Laundry builders and surfactants derived from bio-based hydroxyacids and epoxides
CN106045946A (en) Preparation method of sorbitan tristearate
Sivaramakrishnan The use of surfactants in the finishing of technical textiles
US2751358A (en) Non-foaming detergents
Karis et al. Non‐fuel uses for fatty acid methyl esters
CN102618250A (en) Preparation method of environmental-friendly demulsify-cleanup additive for fracture acidizing
US11597892B2 (en) Method for washing hard article
CN106117167A (en) The preparation method of Arlacel-60
US2189397A (en) Organic nitrogenous base derivatives of ether derivatives
US2369818A (en) Water-soluble high molal oxyalkylated esters, and method of making same
CN108690594A (en) A kind of method of thick-oil emulsified adhesive-reducing

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20180814

CF01 Termination of patent right due to non-payment of annual fee