CN106282443A - A kind of preparation method of phosphate fat-liquoring agent - Google Patents

A kind of preparation method of phosphate fat-liquoring agent Download PDF

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Publication number
CN106282443A
CN106282443A CN201610688686.7A CN201610688686A CN106282443A CN 106282443 A CN106282443 A CN 106282443A CN 201610688686 A CN201610688686 A CN 201610688686A CN 106282443 A CN106282443 A CN 106282443A
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China
Prior art keywords
agent
preparation
adds
leather
phospholipid
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CN201610688686.7A
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CN106282443B (en
Inventor
刘显奎
张健康
张海煊
尹岳涛
闫文飞
石传晋
李幸
曾杰辉
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China Leather and Footwear Research Institute Jinjiang Co Ltd
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China Leather and Footwear Research Institute Jinjiang Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C14SKINS; HIDES; PELTS; LEATHER
    • C14CCHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
    • C14C9/00Impregnating leather for preserving, waterproofing, making resistant to heat or similar purposes
    • C14C9/02Impregnating leather for preserving, waterproofing, making resistant to heat or similar purposes using fatty or oily materials, e.g. fat liquoring
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00Compounds containing elements of Groups 5 or 15 of the Periodic Table
    • C07F9/02Phosphorus compounds
    • C07F9/06Phosphorus compounds without P—C bonds
    • C07F9/08Esters of oxyacids of phosphorus
    • C07F9/09Esters of phosphoric acids
    • C07F9/10Phosphatides, e.g. lecithin
    • C07F9/103Extraction or purification by physical or chemical treatment of natural phosphatides; Preparation of compositions containing phosphatides of unknown structure

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)

Abstract

The invention discloses the preparation method of a kind of phosphate fat-liquoring agent, the phospholipid oils and fats of present invention activation compounds natural soybean phospholipid, wherein uses P2O5The phospholipid of activation can combine with the active group on leather fiber, phospholipid of natural soybean is the most mainly filled between leather fiber, under the conditions of the hydrotropy of organic alcohols solvent, obtain that emulsifiability is good, store stable phosphide class fatting agent, this fatting agent can give the pliability that leather is good, makes leather have the sliding feel of silk and obvious filling effect.

Description

A kind of preparation method of phosphate fat-liquoring agent
Technical field
The invention belongs to leather phosphide class fatting agent, relate to a kind of leather fatting agent and preparation method thereof.
Background technology
Stuffing during leather produces is to process leather under certain process conditions with fatting agent, makes leather absorb a certain amount of Oils and fats and give the process that leather has preferable physical and mechanical properties and serviceability.By chemically and physically acting on, add Fat can make to be full of oils and fats or or fiber surface keyed jointing substantial amounts of " oiliness " molecule, the increasing with lubrication between leather fiber Add interfibrous mutual mobility, thus prevent leather from hardening, jackknifing, and make leather have corresponding elasticity, toughness, extension Property and flexibility.
Fatting agent can be divided into anionic, cationic, nonionic and amphoteric;Can be divided into by the function of fatting agent Impregnating and Fatliquoring Agent, the fatting agent of resistance to light type, flame retardant type fatting agent, retanned fatting agent etc.;Can be divided into by the difference of neutral oil and planting Thing oils and fats fatting agent, animal oil fatting agent, mineral grease fatting agent, synthetic fat liquor, fat liquoring complex agent etc.;By hydrophilic group Difference can be divided into sulphation fatting agent, sulfiting fatting agent, phosphorylation fatting agent etc..Different fatting agents, its function has Different stresses.Traditional phosphide class fatting agent emulsifiability is the best, and bin stability is poor, and needs assist at other fatting agents Under the conditions of use.The complex class phospholipid fatting agent that the present invention relates to, it is possible to be used alone, automatic emulsifying performance is good, and storage is stable, In addition to giving the stuffing effect that leather is soft, also there is good fillibility and the feel of silk cunning.
Summary of the invention
For the problems referred to above, the invention provides the preparation method of a kind of phosphate fat-liquoring agent.
For solving above-mentioned technical problem, the technical solution adopted in the present invention is: the preparation side of a kind of phosphate fat-liquoring agent Method:
The first step: by 50-70kg Oleum Ricini and 30-50kg neat's foot oil, put in the reactor cleaned up, add five oxygen Change two phosphorus 12-15kg, be stirred, carry out temperature reaction 30-50min, be warmed up to 72-75 DEG C, be incubated 1.5-2h, reacted Thing a;
Second step: add 60 DEG C of water 5kg in a, cool to 65-70 DEG C, hydrolysis 1.5h obtains hydrolysate b;
3rd step: potassium hydroxide 15-25kg, after 97kg water dissolution, adds in b, in red after stirring at less than 60 DEG C Brown liquid, while hot discharging, be light yellow paste flowable thing c after cooling;
4th step: take the c of 70%-85%, adds 8%-15% soybean phospholipid and the hydrophilic alcohols of short chain of 11%-13% Compound, by the organic base regulation solution ph of 0.6%-2% to 7.5-8.0, obtains the flowable products d of mixed phosphatide;
5th step: with the working substance content of water adjustment d to 60-70%, obtain phosphide class fatting agent.
Further, the one during described organic base is monoethanolamine, diethanolamine and triethanolamine or mixture.
Further, described short chain hydrophilic polyol compounds is the one in ethylene glycol or diethylene glycol.
From the above-mentioned description to present configuration, compared to the prior art, present invention have the advantage that the present invention Disclosing the preparation method of a kind of phosphate fat-liquoring agent, the phospholipid oils and fats of present invention activation compounds natural soybean phospholipid, Wherein use P2O5The phospholipid of activation can combine with the active group on leather fiber, and phospholipid of natural soybean is then mainly filled Between leather fiber, under the conditions of the hydrotropy of organic alcohols solvent, it is thus achieved that emulsifiability is good, store stable phosphide class Fatting agent, this fatting agent can give the pliability that leather is good, makes leather have the sliding feel of silk and obvious filling effect.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, present invention below is carried out the most in detail Describe in detail bright.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Embodiment 1
The first step: by 50kg Oleum Ricini and 30kg neat's foot oil, puts in the reactor cleaned up, adds phosphorus pentoxide 12kg, is stirred, and carries out temperature reaction 30min, is warmed up to 72 DEG C, is incubated 1.5h, obtains reactant a.
Second step: add 60 DEG C of water 5kg in a, cool to 65 DEG C, hydrolyze 1.5 hours, obtain hydrolysate b.
3rd step: potassium hydroxide 15kg, after 97kg water dissolution, adds in b, in rufous after stirring under less than 60 degree Liquid, while hot discharging, be light yellow paste flowable thing c after cooling.
4th step: take the c of 70%, adds the short chain hydrophilic polyol compounds of 15% soybean phospholipid and 13%, with 2% have Machine alkali regulation solution ph, to 7.5, obtains the flowable products d of mixed phosphatide.
5th step: with the working substance content of water adjustment d to 60%, obtain phosphide class fatting agent.
Organic base used is monoethanolamine, and short chain hydrophilic polyol compounds used is ethylene glycol.
Embodiment 2
The first step: by 60kg Oleum Ricini and 50kg neat's foot oil, puts in the reactor cleaned up, adds phosphorus pentoxide 13kg, is stirred, and carries out temperature reaction 40min, is warmed up to 75 DEG C, is incubated 2h, obtains reactant a.
Second step: add 60 DEG C of water 5kg in a, cool to 65 DEG C, hydrolysis 1.5h obtains hydrolysate b.
3rd step: potassium hydroxide 20kg, after 97kg water dissolution, adds in b, in rufous after stirring at less than 60 DEG C Liquid, while hot discharging, be light yellow paste flowable thing c after cooling.
4th step: take the c of 73%, adds the short chain hydrophilic polyol compounds of 15% soybean phospholipid and 11%, with 1% have Machine alkali regulation solution ph, to 7.5-8.0, obtains the flowable products d of mixed phosphatide.
5th step: with the working substance content of water adjustment d to 65%, obtain phosphide class fatting agent.Organic base used is two Ethanolamine, short chain hydrophilic polyol compounds used is diethylene glycol.
Embodiment 3
The first step: by 65kg Oleum Ricini and 45kg neat's foot oil, puts in the reactor cleaned up, adds phosphorus pentoxide 13kg, is stirred, and carries out temperature reaction 50min, is warmed up to 75 DEG C, is incubated 2h, obtains reactant a.
Second step: add 60 DEG C of water 5kg in a, cool to 70 DEG C, hydrolyze 1.5h, obtain hydrolysate b.
3rd step: potassium hydroxide 22kg, after 97kg water dissolution, adds in b, in rufous after stirring at less than 60 DEG C Liquid, while hot discharging, be light yellow paste flowable thing c after cooling.
4th step: take the c of 78%, adds the short chain hydrophilic polyol compounds of 8% soybean phospholipid and 12%, with 2% have Machine alkali regulation solution ph, to 8.0, obtains the flowable products d of mixed phosphatide.
5th step: with the working substance content of water adjustment d to 62%, obtain phosphide class fatting agent.Organic base used is three Ethanolamine, short chain hydrophilic polyol compounds used is diethylene glycol.
Embodiment 4
The first step: by 68kg Oleum Ricini and 47kg neat's foot oil, puts in the reactor cleaned up, adds phosphorus pentoxide 15kg, is stirred, and carries out temperature reaction 50min, is warmed up to 75 DEG C, is incubated 2h, obtains reactant a.
Second step: add 60 DEG C of water 5kg in a, cool to 70 DEG C, hydrolyze 1.5h, obtain hydrolysate b.
3rd step: potassium hydroxide 23kg, after 97kg water dissolution, adds in b, in rufous after stirring at less than 60 DEG C Liquid, while hot discharging, be light yellow paste flowable thing c after cooling.
4th step: take the c of 80%, adds the short chain hydrophilic polyol compounds of 8% soybean phospholipid and 11%, with 1% have Machine alkali regulation solution ph, to 8.0, obtains the flowable products d of mixed phosphatide.
5th step: with the working substance content of water adjustment d to 68%, obtain phosphide class fatting agent.Organic base used is one Ethanolamine, short chain hydrophilic polyol compounds used is ethylene glycol.
Embodiment 5
The first step: by 70kg Oleum Ricini and 50kg neat's foot oil, puts in the reactor cleaned up, adds phosphorus pentoxide 12kg, is stirred, and carries out temperature reaction 30min, is warmed up to 72 DEG C, is incubated 1.5h, obtains reactant a.
Second step: add 60 DEG C of water 5kg in a, cool to 65 DEG C, hydrolyze 1.5h, obtain hydrolysate b.
3rd step: potassium hydroxide 15kg, after 97kg water dissolution, adds in b, in rufous after stirring at less than 60 DEG C Liquid, while hot discharging, be light yellow paste flowable thing c after cooling.
4th step: take the c of 76%, adds the short chain hydrophilic polyol compounds of 10% soybean phospholipid and 12%, 2% organic Alkali regulation solution ph, to 7.5-8., obtains the flowable products d of mixed phosphatide.
5th step: with the working substance content of water adjustment d to 70%, obtain phosphide class fatting agent.Organic base used is three Ethanolamine, short chain hydrophilic polyol compounds used is ethylene glycol.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.

Claims (3)

1. a preparation method for phosphate fat-liquoring agent, its feature is as follows:
The first step: by 50-70kg Oleum Ricini and 30-50kg neat's foot oil, puts in the reactor cleaned up, and adds five oxidations two Phosphorus 12-15kg, is stirred, and carries out temperature reaction 30-50min, is warmed up to 72-75 DEG C, is incubated 1.5-2h, obtains reactant a;
Second step: add 60 DEG C of water 5kg in a, cool to 65-70 DEG C, hydrolysis 1.5h obtains hydrolysate b;
3rd step: potassium hydroxide 15-25kg, after 97kg water dissolution, adds in b, in rufous after stirring at less than 60 DEG C Liquid, while hot discharging, be light yellow paste flowable thing c after cooling;
4th step: take the c of 70%-85%, adds 8%-15% soybean phospholipid and the short chain hydrophilic alcohols chemical combination of 11%-13% Thing, by the organic base regulation solution ph of 0.6%-2% to 7.5-8.0, obtains the flowable products d of mixed phosphatide;
5th step: with the working substance content of water adjustment d to 60-70%, obtain phosphide class fatting agent.
The preparation method of a kind of phosphate fat-liquoring agent the most according to claim 1, it is characterised in that: described organic base is one One in ethanolamine, diethanolamine and triethanolamine or mixture.
The preparation method of a kind of phosphate fat-liquoring agent the most according to claim 1, it is characterised in that: described short chain hydrophilic polyol Compounds is the one in ethylene glycol or diethylene glycol.
CN201610688686.7A 2016-08-18 2016-08-18 A kind of preparation method of phosphate fat-liquoring agent Active CN106282443B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5391784A (en) * 1987-05-22 1995-02-21 Chemische Fabrik Stockhausen Gmbh Liquid or flowable derivatives of natural fats and oils a process for their production and their use
US5525333A (en) * 1992-05-11 1996-06-11 Solvay Deutschland Gmbh Lactobionic acid amide compositions and their use
CN1382808A (en) * 2001-04-24 2002-12-04 中国科学院成都有机化学研究所 Process for preparing greasing agent
CN1865454A (en) * 2006-04-30 2006-11-22 温州大学 Composite phosphate grease-adding agent for leather and its preparation method
CN104060003A (en) * 2014-07-10 2014-09-24 北京泛博科技有限责任公司 Fatting agent and preparation method thereof
CN105648125A (en) * 2016-03-25 2016-06-08 陕西科技大学 Preparation method of polyhydroxyl-modified soybean phosphatide fatliquoring agent

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5391784A (en) * 1987-05-22 1995-02-21 Chemische Fabrik Stockhausen Gmbh Liquid or flowable derivatives of natural fats and oils a process for their production and their use
US5525333A (en) * 1992-05-11 1996-06-11 Solvay Deutschland Gmbh Lactobionic acid amide compositions and their use
CN1382808A (en) * 2001-04-24 2002-12-04 中国科学院成都有机化学研究所 Process for preparing greasing agent
CN1865454A (en) * 2006-04-30 2006-11-22 温州大学 Composite phosphate grease-adding agent for leather and its preparation method
CN104060003A (en) * 2014-07-10 2014-09-24 北京泛博科技有限责任公司 Fatting agent and preparation method thereof
CN105648125A (en) * 2016-03-25 2016-06-08 陕西科技大学 Preparation method of polyhydroxyl-modified soybean phosphatide fatliquoring agent

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
马建中: "《皮革化学品的合成原理与应用技术》", 31 August 2009 *

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