CN108568348A - A kind of vegetable fatty acid acyl breast ester soap collecting agent and preparation method thereof - Google Patents

A kind of vegetable fatty acid acyl breast ester soap collecting agent and preparation method thereof Download PDF

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Publication number
CN108568348A
CN108568348A CN201810321743.7A CN201810321743A CN108568348A CN 108568348 A CN108568348 A CN 108568348A CN 201810321743 A CN201810321743 A CN 201810321743A CN 108568348 A CN108568348 A CN 108568348A
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CN
China
Prior art keywords
preparation
collecting agent
fatty acid
cotton oil
ester soap
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.)
Pending
Application number
CN201810321743.7A
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Chinese (zh)
Inventor
罗惠华
邹志雄
张振翼
蔡忠俊
刘幸
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Xiaogan Tianxiang Mining Polytron Technologies Inc
Wuhan Institute of Technology
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Xiaogan Tianxiang Mining Polytron Technologies Inc
Wuhan Institute of Technology
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Application filed by Xiaogan Tianxiang Mining Polytron Technologies Inc, Wuhan Institute of Technology filed Critical Xiaogan Tianxiang Mining Polytron Technologies Inc
Priority to CN201810321743.7A priority Critical patent/CN108568348A/en
Publication of CN108568348A publication Critical patent/CN108568348A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • B03D1/004Organic compounds
    • B03D1/008Organic compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11CFATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
    • C11C3/00Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
    • C11C3/003Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fatty acids with alcohols
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/02Collectors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00Specified materials treated by the flotation agents; specified applications
    • B03D2203/02Ores
    • B03D2203/04Non-sulfide ores
    • B03D2203/06Phosphate ores

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)

Abstract

The invention belongs to Collophanite flotation technology, a kind of vegetable fatty acid acyl breast ester soap collecting agent and preparation method thereof is disclosed.The cotton oil aliphatic acid and lactic acid that the present invention is 120 135 using iodine number are mixed progress esterification and saponification successively and obtain the vegetable fatty acid acyl breast ester soap collecting agent as primary raw material;The collecting agent has excellent dissolubility, dispersibility and anti-hardness, and normal temperature flotation effect is good, and collecting ability is strong, stability is good;And the raw material sources that are related to are wide, preparation process is simple, have important dissemination in collophane ore dressing field.

Description

A kind of vegetable fatty acid acyl breast ester soap collecting agent and preparation method thereof
Technical field
The invention belongs to beneficiation reagent technical fields, and in particular to a kind of vegetable fatty acid acyl breast ester soap collecting agent and its system Preparation Method.
Background technology
Phosphorus ore is the essential basic material for producing phosphate fertilizer, fine phosphorus chemical product, is important strategic in China Mineral resources.China's phosphate rock resource rich reserves, but the mostly lower mid low grade phosphate rock of phosphorus content, the Gao Pin that can directly utilize Position rock phosphate in powder is only capable of maintaining more than ten years exploitation.Mid-low grade collophanite ore due to various mineral inlay relationship is complicated, disseminated grain size is thin, Dissociative is poor, while silicate, the features such as carbonate mineral content is high, and utilization belong to global problem.
In phosphate rock floating, existing collecting agent is low in the presence of selectivity, and flotation at low temperature effect is poor, needs to heat flotation and medicine The shortcomings of agent dosage is big causes beneficiation cost higher.
Invention content
The present invention is intended to provide the collophane room temperature that a kind of cryogenic property is excellent, solubility is good, selectivity is strong, collecting ability is strong Direct flotation collecting agent and preparation method thereof.
To achieve the above object, the technical solution adopted by the present invention is:
A kind of vegetable fatty acid acyl breast ester soap collecting agent, based on its cotton oil aliphatic acid and lactic acid with iodine number for 120-135 Raw material is wanted, esterification is carried out successively and saponification forms;The iodine number be 120-135 cotton oil aliphatic acid in respectively composition and Its shared mass content includes:C16:03-4%, C18:04-5%, C18:110-20%, C18:275-85%, C18:32-5%, C16Following content is no more than 2%.
A kind of preparation method of above-mentioned fatty acid acyl breast ester soap collecting agent, includes the following steps:
1) cotton oil aliphatic acid is heated, then the cotton oil aliphatic acid after heating is added in lactic acid, under stirring condition Carry out dehydration esterification reaction;
2) lye is added into step 1) products therefrom, then heating carries out saponification, obtains fatty acid acyl breast ester soap and catches Receive agent.
In said program, the iodine number of the cotton oil aliphatic acid is wherein respectively formed for 120-135 and its shared mass content packet It includes:C16:03-4%, C18:04-5%, C18:110-20%, C18:275-85%, C18:32-5%, C16Following content is no more than 2%.
In said program, the mass ratio of the cotton oil aliphatic acid and lactic acid is 100:(10-40).
In said program, the pH value > 11.5 of the lye.
In said program, the matter of the lye and step 1) products therefrom (in terms of the gross mass of cotton oil aliphatic acid and lactic acid) Amount is than being 1-3:1.
In said program, sodium hydroxide solution or sodium carbonate liquor etc. can be selected in the lye;
Further, the lye selects sodium hydroxide solution;Cotton oil aliphatic acid and the mass ratio of introducing sodium hydroxide are 100:(20-28)。
In said program, the step 1) heating temperature is 80-100 DEG C.
In said program, the temperature of the step 1) dehydration esterification reaction is 80-100 DEG C, time 90-120min.
In said program, the saponification temperature is 70-80 DEG C, reaction time 20-30min.
Chemical equation according to the present invention has:
Aliphatic acid and lactated reaction:
RCOOH+CH3CH (OH) COOH (lactic acid) → RCOOCH (CH3)COOH+H2O
Saponification:
RCOOCH(CH3)COOH+NaOH→RCOOCH(CH3)COONa+H2O
RCOOH+NaOH→RCOONa+H2O
Compared with prior art, beneficial effects of the present invention are:
1) for the present invention using lactic acid and aliphatic ester metaplasia at fatty acid acyl breast ester, the introducing of polar group can improve medicine To the adaptability of temperature, foreign ion etc., reducing dosing makes it show good chemistry within the scope of wider pH for agent Stability, it is excellent disperse, solubilising, thickening and lubricating action;Synergistic effect to fatty acid soaps collecting agent simultaneously, can obviously carry Height reduces the conditions such as the temperature of flotation to the selectivity of phosphorus, shows higher flotation efficiency.
2) raw material sources of the present invention are simple, cheap, and production line is simple, production process is safe, non-stimulated Property smell, reduces beneficiation cost, a new way is provided for efficient flotation process of phosphorite.
Specific implementation mode
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention Content is not limited solely to the following examples.
Embodiment 1
A kind of vegetable fatty acid acyl breast ester soap collecting agent, preparation method include the following steps:
1) the cotton oil aliphatic acid that 100 parts by weight iodine numbers are 120 is weighed, is heated to 80 DEG C;Weigh the breast of 10 parts by weight Acid stirs 30min at 80 DEG C, the cotton oil aliphatic acid after heating is added in lactic acid under agitation, and under the conditions of 80 DEG C Esterification 90min;
2) sodium hydroxide for weighing 22 parts by weight is added in the water of 88 parts by weight, is made into sodium hydroxide solution;Then it is added In reaction product obtained by step 1), saponification 20min under the conditions of 80 DEG C is cooling up to the vegetable fatty acid acyl breast ester soap Collecting agent.
Embodiment 2
A kind of vegetable fatty acid acyl breast ester soap collecting agent, preparation method include the following steps:
1) the cotton oil aliphatic acid that 100 parts by weight iodine numbers are 120 is weighed, is heated to 100 DEG C;Weigh the breast of 20 parts by weight Acid stirs 30min at 100 DEG C, the cotton oil aliphatic acid after heating is added in lactic acid under agitation, and in 100 DEG C of conditions Lower esterification 105min;Be cooled to 80 DEG C it is spare;
2) sodium hydroxide for weighing 24 parts by weight is added in the water of 96 parts by weight, is made into sodium hydroxide solution;Then it is added In reaction product obtained by step 1), saponification 20min under the conditions of 80 DEG C is cooling up to the vegetable fatty acid acyl breast ester soap Collecting agent.
Embodiment 3
A kind of vegetable fatty acid acyl breast ester soap collecting agent, preparation method include the following steps:
1) the cotton oil aliphatic acid that 100 parts by weight iodine numbers are 130 is weighed, is heated to 100 DEG C;Weigh the breast of 30 parts by weight Acid stirs 30min at 100 DEG C, the cotton oil aliphatic acid after heating is added in lactic acid under agitation, and in 100 DEG C of conditions Lower esterification 120min;Be cooled to 80 DEG C it is spare;
2) sodium hydroxide for weighing 26 parts by weight is added in the water of 104 parts by weight, is made into sodium hydroxide solution;Then it is added In reaction product obtained by step 1), saponification 20min under the conditions of 80 DEG C is cooling up to the vegetable fatty acid acyl breast ester soap Collecting agent.
Examples 1 to 3 products therefrom is applied to Sichuan phosphate rock floating and carries out contrast test, the wherein grade of raw ore 21.7% or so, 20 DEG C of flotation temperature passes through one roughing under identical dosing and mog;Gained flotation results are shown in Table 1.
Gained vegetable fatty acid acyl breast ester soap collecting agent of the invention is soluble very well, under equal conditions than fatty acid soaps and Vegetable fatty acid diglycollic amide ester soap compound collecting agent it is more soluble, further show more preferably dispersibility, it is anti-hardness and Collecting performance, and can collecting agent product polar groups obtained by valid certificates introducing.
Collecting agent and the flotation test result of existing fatty acid soaps collecting agent under the same conditions obtained by 1 Examples 1 to 3 of table
Test result shows due to introducing carboxyl (anionic surfactant) while introducing ester group in collecting agent, together When increase carbochain;The introducing of polar group can increase the solubility, the degree of dissociation and salt tolerance of medicament, and the growth of carbochain makes Target minreal surface is more hydrophobic, enhances the collecting ability of medicament.Under same experiment condition with pure oleic acid and raw material cotton oil Acid is compared, and anionic mixed type vegetable fatty acid acyl breast ester soap flotation agent has preferable dissolubility, dispersibility and anti-hardness, Normal temperature flotation effect is preferable, and collecting ability is strong, and higher by phosphorus concentrate grade obtained by roughing, the rate of recovery is also higher, aeneficiation effect There is larger improvement.For comparing vegetable fatty acid diglycollic amide ester soap compounding collecting agent, the rate of recovery can be improved 4.77%, ore dressing Efficiency can promote 3.75% and (be equivalent to the 52.2% of vegetable fatty acid diglycollic amide ester soap compounding collecting agent beneficiating efficiency, increase Long amplitude is up to 50% or more).
In conclusion vegetable fatty acid acyl breast ester soap collecting agent has preferable dissolubility, dispersibility and anti-hardness, room temperature floating Select effect preferable, collecting ability is strong and synthesis material is easily purchased, cheap, and production line is simple, production process is safe, stingless Swash property smell, reduces beneficiation cost, overcome the deficiencies in the prior art, there is certain promotion price for flotation of phosphate rock industry Value.
Particular embodiments described above has carried out further the purpose of the present invention, technical solution and advantageous effect It is described in detail.For those skilled in the art, the present invention can have various modifications and variations, all spirit in the present invention With any modification made in principle, equivalent replacement, improvement etc. should all be in protection scope of the present invention.

Claims (10)

1. a kind of vegetable fatty acid acyl breast ester soap collecting agent, which is characterized in that it with iodine number for 120-135 cotton oil aliphatic acid and Lactic acid is primary raw material, carries out esterification successively and saponification forms.
2. a kind of preparation method of fatty acid acyl breast ester soap collecting agent, which is characterized in that include the following steps:
1) cotton oil aliphatic acid is heated, then the cotton oil aliphatic acid after heating is added in lactic acid, is carried out under stirring condition Dehydration esterification reaction;
2) lye is added into step 1) products therefrom, then heating carries out saponification, obtains fatty acid acyl breast ester soap collecting agent.
3. preparation method according to claim 2, which is characterized in that the iodine number of the cotton oil aliphatic acid is 120-135.
4. preparation method according to claim 2, which is characterized in that the mass ratio of the cotton oil aliphatic acid and lactic acid is 100:(10-40)。
5. preparation method according to claim 2, which is characterized in that the lye is sodium hydroxide or sodium carbonate liquor.
6. preparation method according to claim 2, which is characterized in that the pH value > 11.5 of the lye.
7. preparation method according to claim 2, which is characterized in that the mass ratio of the lye and step 1) products therefrom For (1-3):1.
8. preparation method according to claim 2, which is characterized in that the step 1) heating temperature is 80-100 DEG C.
9. preparation method according to claim 2, which is characterized in that the temperature of the step 1) dehydration esterification reaction is 80-100 DEG C, time 90-120min.
10. preparation method according to claim 2, which is characterized in that the saponification temperature is 70-80 DEG C, reaction Time is 20-30min.
CN201810321743.7A 2018-04-11 2018-04-11 A kind of vegetable fatty acid acyl breast ester soap collecting agent and preparation method thereof Pending CN108568348A (en)

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109894282A (en) * 2019-03-25 2019-06-18 甘肃有色冶金职业技术学院 A method of low-grade phosphate ore direct flotation collecting agent is prepared based on Converted From Crushed Vegetable Oil Scrap
CN110280392A (en) * 2019-07-15 2019-09-27 宜都兴发化工有限公司 A kind of preparation method of vegetable fatty acid galla turcica ester collecting agent

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104874487A (en) * 2015-06-03 2015-09-02 武汉工程大学 Preparation method of plant fatty acid and alkyl citrate soap compound collecting agent
CN106076649A (en) * 2016-05-20 2016-11-09 孝感市天翔矿业科技有限公司 A kind of fatty acid apple ester soap collecting agent preparation method
CN106622671A (en) * 2016-12-27 2017-05-10 中蓝连海设计研究院 Direct flotation desiliconization and acid leaching magnesium removal combination treatment technology for phosphate ores

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104874487A (en) * 2015-06-03 2015-09-02 武汉工程大学 Preparation method of plant fatty acid and alkyl citrate soap compound collecting agent
CN106076649A (en) * 2016-05-20 2016-11-09 孝感市天翔矿业科技有限公司 A kind of fatty acid apple ester soap collecting agent preparation method
CN106622671A (en) * 2016-12-27 2017-05-10 中蓝连海设计研究院 Direct flotation desiliconization and acid leaching magnesium removal combination treatment technology for phosphate ores

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
罗廉明等: "一种新型磷矿浮选捕收剂", 《武汉化工学院学报》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109894282A (en) * 2019-03-25 2019-06-18 甘肃有色冶金职业技术学院 A method of low-grade phosphate ore direct flotation collecting agent is prepared based on Converted From Crushed Vegetable Oil Scrap
CN110280392A (en) * 2019-07-15 2019-09-27 宜都兴发化工有限公司 A kind of preparation method of vegetable fatty acid galla turcica ester collecting agent

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