CN1837177A - Process for preparing alpha-zinc linolenate - Google Patents
Process for preparing alpha-zinc linolenate Download PDFInfo
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- CN1837177A CN1837177A CN 200510107354 CN200510107354A CN1837177A CN 1837177 A CN1837177 A CN 1837177A CN 200510107354 CN200510107354 CN 200510107354 CN 200510107354 A CN200510107354 A CN 200510107354A CN 1837177 A CN1837177 A CN 1837177A
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- linolenic acid
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Abstract
The invention relates to a process for preparing alpha-zinc linolenate by using perilla oil as the raw material, which comprises the steps of saponifying, neutralizing, double decomposition, stewing, scouring, dewatering and drying. The obtained alpha-zinc linolenate has higher content of alpha-linolenic acid.
Description
Technical field
The present invention relates to a kind of is the preparation method of raw material production alpha-linolenic acid zinc with the perilla oil.
Background technology
Alpha-linolenic acid mainly is present in the various plants grease with the triglyceride level form, comprise linseed oil, Purple Perilla Seed Oil, rape seed oil, Oleum Gossypii semen, soybean wet goods, wherein content is up to 50%～60% in linseed oil, the Purple Perilla Seed Oil, and content is all below 10% in other oil.To unsaturated fatty acids famine, particularly alpha-linolenic acid, need to replenish among the crowd from other approach.In medicine, food service industry, how to use, generally lack zinc in addition among the crowd, make the combination of alpha-linolenic acid and zinc, make the crowd replenish alpha-linolenic acid and zinc preferably as adding, and the domestic present not preparation method of invention alpha-linolenic acid zinc.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art and the preparation method of the also big alpha-linolenic acid zinc of a kind of content that not only contains a large amount of alpha-linolenic acids and zinc is provided.
The object of the present invention is achieved like this: carry out according to following technology:
The first step: saponification: perilla oil and the deionized water ratio by weight 1: 0.5～4 is added in the container; stir and heating, control material reaction temperature slowly adds 5%～30% ionic membrane caustic soda between 40 ℃～90 ℃; when the material pH value greater than 12 the time; stop to add ionic membrane caustic soda, when the material pH value less than 10 the time, slowly add ionic membrane caustic soda; when the material pH value keeps 2 hours when constant greater than 10; reaction finishes, the omnidistance logical nitrogen protection of this operation
Second step: neutralization: add in container and stirring in 1: 3～10 ratio the first step gained material, deionized water weight ratio; obtain milky white solution, slowly add 30%～90% sulfuric acid milky white solution is neutralized to PH=7, this operation finishes; the omnidistance logical nitrogen protection of this operation
The 3rd step: metathesis: zinc sulfate, deionized water are configured to solution of zinc sulfate by weight 1: 4～10 ratio adding container and stirring; the second step gained material and solution of zinc sulfate are added in the container; control reaction temperature is between 40 ℃～90 ℃; stir; 1～3 hour time can produce a large amount of dispersive white floss---alpha-linolenic acid zinc, and this operation finishes; the omnidistance logical nitrogen protection of this operation
The 4th step: leave standstill: the 3rd step gained material is left standstill in container, and temperature is controlled between 40～90 ℃, left standstill 6～10 hours,
The 5th step: washing: discharge the aqueous solution in the 4th step gained material, add deionized water white alpha-linolenic acid zinc floss is washed, drainage water solution repeats aforesaid operations, and is as clear as crystal until the aqueous solution of discharging,
The 6th step: dehydration: the 5th step gained material is put into whizzer, carry out centrifuge dehydration, make alpha-linolenic acid zinc and water realize solid-liquid separation,
The 7th step: drying:, promptly get little yellow solid alpha-linolenic acid zinc with the 6th step gained solid materials under 40～90 ℃, vacuum 400～700mmHg condition dry 20～35 hours.
The present invention has following positively effect:
The first, the present invention has successfully realized the preparation of alpha-linolenic acid zinc.
The second, make the interpolation approach of alpha-linolenic acid more extensive.
Three, make the crowd better replenish alpha-linolenic acid and zinc, promoted that effectively the crowd is healthy.
Four, the alpha-linolenic acid content height of the alpha-linolenic acid zinc of the present invention's preparation, alpha-linolenic acid content is greater than 55%, and the content of zinc is greater than 6%, and all other indexs meet the provisions of the relevant regulations issued by the State.
Embodiment
Embodiment 1:
The first step: saponification: perilla oil 100 grams and deionized water 50 grams are added in the container; stir and heating, 40 ℃ of control material reaction temperature slowly add 5% ionic membrane caustic soda; when the material pH value greater than 12 the time; stop to add ionic membrane caustic soda, when the material pH value less than 10 the time, slowly add ionic membrane caustic soda; keep greater than 10 when the material pH value and to keep 2 hours when constant; reaction finishes, the omnidistance logical nitrogen protection of this operation
Second step: neutralize: add in the containers the first step gained material 450 grams, deionized water 1350 grams and stirring, obtain milky white solution, slowly add 30% sulfuric acid milky white solution is neutralized to PH=7, this operation finishes, the omnidistance logical nitrogen protection of this operation,
The 3rd step: metathesis: be configured to solution of zinc sulfate with also stirring in zinc sulfate 100 grams, the deionized water 400 gram adding containers; the second step gained material and solution of zinc sulfate are added in the container; 40 ℃ of control reaction temperature; stir; 1 hour time can produce a large amount of dispersive white floss---alpha-linolenic acid zinc, and this operation finishes; the omnidistance logical nitrogen protection of this operation
The 4th step: leave standstill: the 3rd step gained material is left standstill in container, and 40 ℃ of temperature controls were left standstill 6 hours,
The 5th step: washing: discharge the aqueous solution in the 4th step gained material, add deionized water white alpha-linolenic acid zinc floss is washed, drainage water solution repeats aforesaid operations, and is as clear as crystal until the aqueous solution of discharging,
The 6th step: dehydration: the 5th step gained material is put into whizzer, carry out centrifuge dehydration, make alpha-linolenic acid zinc and water realize solid-liquid separation,
The 7th step: drying:, promptly get little yellow solid alpha-linolenic acid zinc 5 and restrain with the 6th step gained solid materials under 40 ℃, vacuum 400mmHg condition dry 20 hours.
Embodiment 2:
The first step: saponification: perilla oil 100 grams and deionized water 400 grams are added in the container; stir and heating, 90 ℃ of control material reaction temperature slowly add 30% ionic membrane caustic soda; when the material pH value greater than 12 the time; stop to add ionic membrane caustic soda, when the material pH value less than 10 the time, slowly add ionic membrane caustic soda; when the material pH value keeps 2 hours when constant greater than 10; reaction finishes, the omnidistance logical nitrogen protection of this operation
Second step: neutralize: add in the containers the first step gained material 600 grams, deionized water 6000 grams and stirring, obtain milky white solution, slowly add 90% sulfuric acid milky white solution is neutralized to PH=7, this operation finishes, the omnidistance logical nitrogen protection of this operation,
The 3rd step: metathesis: be configured to solution of zinc sulfate with also stirring in zinc sulfate 100 grams, the deionized water 1000 gram adding containers; the second step gained material and solution of zinc sulfate are added in the container; 90 ℃ of control reaction temperature; stir; 3 hours time can produce a large amount of dispersive white floss---alpha-linolenic acid zinc, and this operation finishes; the omnidistance logical nitrogen protection of this operation
The 4th step: leave standstill: the 3rd step gained material is left standstill in container, and 90 ℃ of temperature controls were left standstill 10 hours,
The 5th step: washing: discharge the aqueous solution in the 4th step gained material, add deionized water white alpha-linolenic acid zinc floss is washed, drainage water solution repeats aforesaid operations, and is as clear as crystal until the aqueous solution of discharging,
The 6th step: dehydration: the 5th step gained material is put into whizzer, carry out centrifuge dehydration, make alpha-linolenic acid zinc and water realize solid-liquid separation,
The 7th step: drying:, promptly get little yellow solid alpha-linolenic acid zinc 6 and restrain with the 6th step gained solid materials under 90 ℃, vacuum 700mmHg condition dry 35 hours.
Embodiment 3:
The first step: saponification: perilla oil 100 grams and deionized water 200 grams are added in the container; stir and heating, 60 ℃ of control material reaction temperature slowly add 20% ionic membrane caustic soda; when the material pH value greater than 12 the time; stop to add ionic membrane caustic soda, when the material pH value less than 10 the time, slowly add ionic membrane caustic soda; keep greater than 10 when the material pH value and to keep 2 hours when constant; reaction finishes, the omnidistance logical nitrogen protection of this operation
Second step: neutralization: the first step gained material 380, deionized water 1900 are restrained to add in the containers and also stir, obtain milky white solution, slowly add 80% sulfuric acid milky white solution is neutralized to PH=7, this operation finishes, the logical nitrogen protection of this operation whole process,
The 3rd step: metathesis; Be configured to solution of zinc sulfate with also stirring in zinc sulfate 100 grams, the deionized water 500 gram adding containers; the second step gained material and solution of zinc sulfate are added in the container; between 80 ℃ of the control reaction temperature; stir; 2 hours time can produce a large amount of dispersive white floss---alpha-linolenic acid zinc, and this operation finishes; the omnidistance logical nitrogen protection of this operation
The 4th step: leave standstill: the 3rd step gained material is left standstill in container, and 50 ℃ of temperature controls were left standstill 8 hours,
The 5th step: washing: discharge the aqueous solution in the 4th step gained material, add deionized water white alpha-linolenic acid zinc floss is washed, drainage water solution repeats aforesaid operations, and is as clear as crystal until the aqueous solution of discharging,
The 6th step: dehydration: the 5th step gained material is put into whizzer, carry out centrifuge dehydration, make alpha-linolenic acid zinc and water realize solid-liquid separation,
The 7th step: drying:, promptly get little yellow solid alpha-linolenic acid zinc 5 and restrain with the 6th step gained solid materials under 60 ℃, vacuum 500mmHg condition dry 25 hours.
Claims (1)
1, a kind of preparation method of alpha-linolenic acid calcium zinc is characterized in that: carry out according to following technology:
The first step: saponification: perilla oil and the deionized water ratio by weight 1: 0.5～4 is added in the container; stir and heating, control material reaction temperature slowly adds 5%～30% ionic membrane caustic soda between 40 ℃～90 ℃; when the material pH value greater than 12 the time; stop to add ionic membrane caustic soda, when the material pH value less than 10 the time, slowly add ionic membrane caustic soda; when the material pH value greater than 10 and keep 2 hours when constant; reaction finishes, the omnidistance logical nitrogen protection of this operation
Second step: neutralization: the first step gained material, deionized water are also stirred in 1: 3～10 ratio adding container; obtain milky white solution, slowly add 30%～90% sulfuric acid milky white solution is neutralized to PH=7, this operation finishes; the omnidistance logical nitrogen protection of this operation
The 3rd step: metathesis: zinc sulfate, deionized water are configured to solution of zinc sulfate by weight 1: 4～10 ratio adding container and stirring; the second step gained material and solution of zinc sulfate are added in the container; control reaction temperature is between 40 ℃～90 ℃; stir; 1～3 hour time produced a large amount of dispersive white floss---linolenic acid zinc, and this operation finishes; the omnidistance logical nitrogen protection of this operation
The 4th step: leave standstill: the 3rd step gained material is left standstill in container, and temperature is controlled between 40～90 ℃, left standstill 6～10 hours,
The 5th step: washing: discharge the aqueous solution in the 4th step gained material, add deionized water white linolenic acid zinc floss is washed, drainage water solution repeats aforesaid operations, and is as clear as crystal until the aqueous solution of discharging,
The 6th step: dehydration: the 5th step gained material is put into whizzer, carry out centrifuge dehydration, make linolenic acid zinc and water realize solid-liquid separation,
The 7th step: drying:, promptly get solid alpha-linolenic acid zinc with the 6th step gained solid materials under 40～90 ℃, vacuum 400～700mmHg condition dry 20～35 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101073547A CN100363324C (en) | 2005-12-30 | 2005-12-30 | Process for preparing alpha-zinc linolenate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101073547A CN100363324C (en) | 2005-12-30 | 2005-12-30 | Process for preparing alpha-zinc linolenate |
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| Publication Number | Publication Date |
|---|---|
| CN1837177A true CN1837177A (en) | 2006-09-27 |
| CN100363324C CN100363324C (en) | 2008-01-23 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2005101073547A Expired - Fee Related CN100363324C (en) | 2005-12-30 | 2005-12-30 | Process for preparing alpha-zinc linolenate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108623448A (en) * | 2018-05-15 | 2018-10-09 | 南京医科大学 | The preparation of leukotrienes zinc and its application in preparing Anti-helicobacter pylori drugs |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1098072C (en) * | 1998-05-12 | 2003-01-08 | 李文光 | Medicinal products of superfined alpha-linolenic acid, preparing process and preparation thereof |
| CN1270160A (en) * | 1999-04-14 | 2000-10-18 | 李文光 | Refined unsaturated polyfatty acid and calcium salt of unsaturated polyfatty acid as medicinal products and preparing process thereof and preparation |
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2005
- 2005-12-30 CN CNB2005101073547A patent/CN100363324C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108623448A (en) * | 2018-05-15 | 2018-10-09 | 南京医科大学 | The preparation of leukotrienes zinc and its application in preparing Anti-helicobacter pylori drugs |
| WO2019219093A3 (en) * | 2018-05-15 | 2019-12-19 | 南京医科大学 | Preparation of zinc linoleate, and application thereof in preparing anti-helicobacter pylori drug |
| US11203563B2 (en) | 2018-05-15 | 2021-12-21 | Nanjing Medical University | Preparation of zinc linolenate, and application of zinc linolenate in preparing anti-helicobacter pylori drug |
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| Publication number | Publication date |
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| CN100363324C (en) | 2008-01-23 |
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