CN1037273A - A kind of production method of producing the peaceful former powder of periodontal - Google Patents
A kind of production method of producing the peaceful former powder of periodontal Download PDFInfo
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- CN1037273A CN1037273A CN89100849A CN89100849A CN1037273A CN 1037273 A CN1037273 A CN 1037273A CN 89100849 A CN89100849 A CN 89100849A CN 89100849 A CN89100849 A CN 89100849A CN 1037273 A CN1037273 A CN 1037273A
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Abstract
A kind of production method of producing the peaceful former powder of periodontal, with Testa oryzae oil alkali refining soap stock behind the methanol alkaline reaction, the filtering residue that extracts before the oryzanol is raw material, carry out water with sodium hydroxide and be saponified into soda soap.Add calcium chloride and make calcium soap, calcium soap is used acetone extract after washing, oven dry, and extract promptly gets the peaceful former powder of periodontal behind layering, precipitation.The present invention has found cheap raw material for the production of the peaceful former powder of periodontal, adopts the single solvent single extraction, has reduced production cost, and has made production operation easy.Also be applicable to that in accordance with the present production process recovered acid carburetion and their residue that Testa oryzae oil alkali refining soap stock, Testa oryzae oil extract behind the oryzanol are raw materials for production.
Description
The present invention relates to oil and fat chemical, relevant with Testa oryzae oil non-saponifiable matter extraction process, the particularly production technology of the peaceful former powder of periodontal.The peaceful former powder of periodontal be a kind ofly contain that non-saponifiable matter is not less than 90%, sterol is not less than 60% refining non-saponifiable matter, is used to cure mainly the important drugs raw material of periodontal.
At present, the production technology of the peaceful former powder of periodontal is to be raw materials for production with Testa oryzae oil two road alkali refining soap stocks, by adding the aqueous solution of methanol and sodium hydroxide, carries out the complete mutually saponification of alcohol under methanol eddy, evaporation reclaim behind the methanol paste of soap (soda soap).Soda soap solvent petroleum ether extraction, extract methanol aqueous solution cyclic washing, standing demix.The layering clear liquid washes with water to being neutral, and revaporization removes petroleum ether, gets thick non-saponifiable matter.Thick non-saponifiable matter solvent methanol reflux extraction, standing demix, extracting and demixing repeats for several times.Methanol extraction layering clear liquid removes solvent methanol through evaporation, and making refining non-saponifiable matter is the peaceful former powder of periodontal.And the actual production of above-mentioned technology, often extracting oryzanol production with Testa oryzae oil again combines, be that Testa oryzae oil alkali refining soap stock is through methanol alkaline reaction after-filtration, filtering residue is that refuse abandons, and filtrate transferring to extracted oryzanol after being faintly acid, and extracts the recovered acid carburetion behind the oryzanol, the raw material of producing as the peaceful former powder of periodontal then, equally, soap stock recited above and recovered acid carburetion also have extracts fatty acid earlier, and reuse is made the raw material that the peaceful former powder of periodontal is produced.
This with the saponification of methanol alkali liquor, petroleum ether extraction, the methanol aqueous solution washing, the extraction process of the peaceful former powder of the purified periodontal of methanol extraction needs with two kinds of solvents, evaporates precipitation several times, and solvent and thermal energy consumption are more, and cost is higher.
The purpose of this invention is to provide a kind of refuse that utilizes in the production of Testa oryzae oil extraction oryzanol, and reduce solvent loss, the production method of producing the peaceful former powder of periodontal easy and simple to handle.
Production method of the present invention be with Testa oryzae oil alkali refining soap stock behind the methanol alkaline reaction, the filtering residue that extracts before the oryzanol is raw material, is soda soap with sodium hydroxide with the saponification of raw material water, add calcium chloride and make calcium soap, calcium soap is used acetone extract after washing, oven dry, the extract layering gets the peaceful former powder of periodontal behind the layering clear liquid precipitation.
Production method of the present invention, raw material also can be any of following material:
1, Testa oryzae oil alkali refining soap stock;
2, the residue behind the Testa oryzae oil alkali refining soap stock extraction fatty acid;
3, the recovered acid carburetion behind the Testa oryzae oil extraction oryzanol;
4; Testa oryzae oil extracts the recovered acid carburetion behind the oryzanol, the residue after extracting fatty acid.
According to the present invention, the refuse that utilizes Testa oryzae oil to extract in the oryzanol production is raw material, carries out the production method of single solvent single extraction, thereby reduced solvent loss significantly, save the energy, reduced production cost, also saved the production investment of solvent evaporation retracting device.
Production method of the present invention is as follows:
1, raw material adds sodium hydroxide and carries out water and be saponified into soda soap.Concentration of lye is 10～30%, and consumption is 0.5～2.5 times of raw material (weight) amount, and saponification temperature is 60～160 ℃, saponification time 2～20 hours.
2, after soda soap is reduced to room temperature, emit alkali and analyse waste water, after adding proper amount of clear water again and stirring, add calcium chloride water, water-soluble heating, generate the particulate calcium soap, after filtration, wash, dry to moisture and be not more than 3%, calcium chloride concentration is 10～25%, consumption is 15～70% of raw material (weight) amount, 40～100 ℃ of reaction temperatures, 1～6 hour time; The calcium soap bake out temperature is 40～70 ℃, 10～40 hours time.
3, exsiccant calcium soap powder extracts with acetone.The acetone consumption is 2～20 times of calcium soap powder (weight) amount, and extraction temperature is 40～60 ℃, 0.5～5 hour time.
4, extract is got the heating of layering clear liquid and is removed solvent acetone through leaving standstill the precipitating layering, gets the peaceful former powder of periodontal.
Embodiment 1:
Take by weighing Testa oryzae oil alkali refining soap stock behind the methanol alkaline reaction, extract the preceding filtering residue of oryzanol 1200 grams, place the saponification device, add the suitable quantity of water dilution and stir well, add concentration 18%.Sodium hydroxide 1400 grams 90 ℃ of following saponification 8 hours, are reduced to room temperature, emit alkali and analyse waste water.Add proper amount of clear water again, stir well the aqueous solution that back adding 400 gram calcium chloride and 1000 gram water are made into, be warming up to 70～80 ℃, reacted 3 hours, blowing, washing, oven dry must be done calcium soap powder 800 grams.
Take by weighing dried calcium soap powder 300 grams, add 1500 milliliters in acetone, boiling extraction 1 hour, homoiothermic is left standstill, and removes the supernatant, again re-extract 1 or 2 times.The extraction clear liquid merges, and steams and take off acetone, gets peaceful former powder 45 grams of periodontal, yield 15%.Mass analysis data is: unsaponifiable matter content is 97.8%, and sterol content is 66.0%, acid number 0.75, and saponification number 1.98, volatile weight loss is 0.52%.All project all meets the peaceful former powder standards of pharmacopoeia of periodontal.
Embodiment 2:
Take by weighing example 1 gained calcium soap 300 grams, add 2000 milliliters in acetone, extracted 2 hours, leave standstill, remove the supernatant, re-extract is 1 to 2 time again.The supernatant merges, evaporative removal acetone, and residue 51.6 grams are 17.2% to the yield of the calcium soap that feeds intake.Analysis result: unsaponifiable matter content is 99.06%, and sterol content is 67.84%, acid number 0.65, and saponification number is 2.18, and volatile weight loss is 0.33%, and its quality meets the peaceful standard of periodontal.
Embodiment 3:
Take by weighing recovered acid carburetion 1000 grams after Testa oryzae oil extracts oryzanol, place the saponification device, add sodium hydroxide 1500 grams of concentration 12%, stirred down heating in water bath 15 hours, put cold spending the night.Emit the bottom alkali waste water.Add low amounts of water, stir, add concentration 25% calcium chloride 2000 grams, heat up, see branch water after, emit filtration, washing, oven dry.Must do calcium soap 960 grams.
Take by weighing calcium soap 400 grams, add 2000 milliliters in acetone.Stir down that heating in water bath refluxed 2 hours, homoiothermic, leave standstill precipitating, tell the supernatant.Re-extract once, twice extraction clear liquid merges, steam in the water-bath and take off acetone, the vacuum precipitation, peaceful former powder 26.3 grams of periodontal.
Embodiment 4:
Take by weighing Testa oryzae oil alkali refining soap stock 1000 grams, add concentration 10% sodium hydroxide 1800 grams, cold spending the night put in agitating heating saponification 9 hours.Discard alkali and analyse waste water.Under agitation add concentration 20% calcium chloride 2500 grams, heating in water bath 3 hours, temperature is 70～75 ℃ eventually, and the elimination clear water is washed to neutrality behind the granulating, oven dry.Must do calcium soap 780 grams.
Take by weighing calcium soap 400 grams, add 2000 milliliters in acetone, stir heating in water bath reflux extraction down 1.5 hours, water-bath stops heating, left standstill precipitating 3 hours, and told the supernatant, re-extract 1 time, twice clear liquid merges, and puts heating in the water-bath, steams and take off acetone, vacuum drying, gets peaceful former powder 45.5 grams of periodontal.
Equally, production method of the present invention, also recovered acid carburetion the residue through extract aliphatic acid after of available rice bran oil alkali refining soap stock behind the residue behind the extraction aliphatic acid or rice bran oil extraction oryzanol is raw materials for production, makes the peaceful former powder of periodontal.
Claims (7)
1, a kind of production method of producing the peaceful former powder of periodontal, with the raw material saponification for receiving soap, add solvent extraction, extract layering, layering clear liquid precipitation, it is characterized in that: with Testa oryzae oil alkali refining soap stock behind the methanol alkaline reaction, extracting the preceding filtering residue of oryzanol is raw material,, adds calcium chloride and makes calcium soap the saponification of filtering residue water with sodium hydroxide, calcium soap is used acetone extract after washing, oven dry, extract gets the peaceful former powder of periodontal behind layering, precipitation.
2, a kind of production method of producing the peaceful former powder of periodontal, rice material rice oil alkali refining soap stock or this soap stock are extracted residue behind the fatty acid or Testa oryzae oil to be extracted recovered acid carburetion behind the oryzanol or this recovered acid carburetion and extracts residue behind the fatty acid and be saponified into and receive soap, add solvent extraction, the extract layering, layering clear liquid precipitation, it is characterized in that: raw material adds calcium chloride and makes calcium soap with the saponification of sodium hydroxide water, and calcium soap is used acetone extract after washing, oven dry.Extract gets the peaceful former powder of periodontal behind layering, precipitation.
3, by claim 1 or 2 described production methods, it is characterized in that: naoh concentration is 10～30%, and consumption is 0.5～2.5 times of raw material (weight) amount.
4, by claim 1 or 2 described production methods, it is characterized in that: calcium chloride concentration is 10～25%, and consumption is 15～70% of raw material (weight) amount, and reaction temperature is 40～100 ℃.
5, by claim 1 or 2 or 4 described production methods, it is characterized in that: calcium soap drying moisture content is less than 3%.
6, by claim 1 or 2 or 4 described production methods, it is characterized in that: the acetone consumption is 2～20 times of calcium soap (weight) amount.
7, by the described production method of claim 5, it is characterized in that: the acetone consumption is 2～20 times of calcium soap (weight) amount.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN89100849A CN1025587C (en) | 1989-02-14 | 1989-02-14 | Production method for preparing periodontitis raw powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN89100849A CN1025587C (en) | 1989-02-14 | 1989-02-14 | Production method for preparing periodontitis raw powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1037273A true CN1037273A (en) | 1989-11-22 |
| CN1025587C CN1025587C (en) | 1994-08-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN89100849A Expired - Fee Related CN1025587C (en) | 1989-02-14 | 1989-02-14 | Production method for preparing periodontitis raw powder |
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| Country | Link |
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| CN (1) | CN1025587C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250692A (en) * | 2011-06-22 | 2011-11-23 | 河南工业大学 | Desolventizing method of soapstock generated during mixed oil refining |
-
1989
- 1989-02-14 CN CN89100849A patent/CN1025587C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250692A (en) * | 2011-06-22 | 2011-11-23 | 河南工业大学 | Desolventizing method of soapstock generated during mixed oil refining |
| CN102250692B (en) * | 2011-06-22 | 2012-12-19 | 河南工业大学 | Desolventizing method of soapstock generated during mixed oil refining |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1025587C (en) | 1994-08-10 |
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