CN101439940A - Technological process for calcining gypsum - Google Patents
Technological process for calcining gypsum Download PDFInfo
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- CN101439940A CN101439940A CNA2008102433026A CN200810243302A CN101439940A CN 101439940 A CN101439940 A CN 101439940A CN A2008102433026 A CNA2008102433026 A CN A2008102433026A CN 200810243302 A CN200810243302 A CN 200810243302A CN 101439940 A CN101439940 A CN 101439940A
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- 229910052602 gypsum Inorganic materials 0.000 title claims abstract description 56
- 239000010440 gypsum Substances 0.000 title claims abstract description 56
- 238000001354 calcination Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims description 25
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000011835 investigation Methods 0.000 claims abstract description 10
- 238000004458 analytical method Methods 0.000 claims abstract description 7
- 229910052925 anhydrite Inorganic materials 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims 1
- 235000010216 calcium carbonate Nutrition 0.000 claims 1
- 230000018044 dehydration Effects 0.000 claims 1
- 238000006297 dehydration reaction Methods 0.000 claims 1
- 238000013386 optimize process Methods 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 17
- 238000012545 processing Methods 0.000 abstract description 10
- 235000011132 calcium sulphate Nutrition 0.000 abstract description 3
- 238000011156 evaluation Methods 0.000 abstract description 3
- 239000001175 calcium sulphate Substances 0.000 abstract description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract 1
- 229910052791 calcium Inorganic materials 0.000 abstract 1
- 239000011575 calcium Substances 0.000 abstract 1
- 238000005242 forging Methods 0.000 description 12
- 238000004062 sedimentation Methods 0.000 description 11
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 description 10
- 239000003814 drug Substances 0.000 description 10
- 239000011507 gypsum plaster Substances 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 210000000697 sensory organ Anatomy 0.000 description 3
- 210000002784 stomach Anatomy 0.000 description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- 229940087511 calcium disodium versenate Drugs 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 235000012907 honey Nutrition 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 210000004072 lung Anatomy 0.000 description 2
- 239000011505 plaster Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 206010011224 Cough Diseases 0.000 description 1
- 235000015001 Cucumis melo var inodorus Nutrition 0.000 description 1
- 240000002495 Cucumis melo var. inodorus Species 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- 208000000059 Dyspnea Diseases 0.000 description 1
- 206010013975 Dyspnoeas Diseases 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- 208000003251 Pruritus Diseases 0.000 description 1
- 208000001431 Psychomotor Agitation Diseases 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 206010038743 Restlessness Diseases 0.000 description 1
- 206010053476 Traumatic haemorrhage Diseases 0.000 description 1
- 208000025865 Ulcer Diseases 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- 208000010668 atopic eczema Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- DEGAKNSWVGKMLS-UHFFFAOYSA-N calcein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC(CN(CC(O)=O)CC(O)=O)=C(O)C=C1OC1=C2C=C(CN(CC(O)=O)CC(=O)O)C(O)=C1 DEGAKNSWVGKMLS-UHFFFAOYSA-N 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229940126678 chinese medicines Drugs 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
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- CEQFOVLGLXCDCX-WUKNDPDISA-N methyl red Chemical compound C1=CC(N(C)C)=CC=C1\N=N\C1=CC=CC=C1C(O)=O CEQFOVLGLXCDCX-WUKNDPDISA-N 0.000 description 1
- 230000001114 myogenic effect Effects 0.000 description 1
- 229960002378 oftasceine Drugs 0.000 description 1
- 238000001543 one-way ANOVA Methods 0.000 description 1
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- 230000001717 pathogenic effect Effects 0.000 description 1
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- 206010036067 polydipsia Diseases 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
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- 238000012216 screening Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 208000004371 toothache Diseases 0.000 description 1
- 231100000397 ulcer Toxicity 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
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- 239000000052 vinegar Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses optimum processing technology for gypsum. The optimum processing technology for the gypsum comprises the following steps: (1) crushing the gypsum into small pieces and placing the crushed gypsum into a crucible; (2) selecting four investigation factors, namely the crushing granularity, the calcining temperature, the calcining time and the laying thickness, and selecting an L18(3<7>) orthogonal table to calcine the crushed gypsum; (3) measuring the hardness, the density, the porocity, the water loss percentage and the CaSO4 content of the calcined gypsum; and (4) performing variance analysis on measuring results, to obtain the optimum processing technology for the gypsum, namely the gypsum is crushed into the small pieces with the granularity of 0.125 cubic centimeter, laid to the thickness of 1 centimeter, and calcined for 1.5 hours at a temperature of 650 DEG C. The optimum processing technology for the gypsum is characterized in that the relative hardness, the relative density, the porocity, the water loss percentage and the calcium content are taken as evaluation indexes of the calcined gypsum; the obtained calcined gypsum is incompact and crisp; the mean water loss percentage is 20.83 percent; the mean relative density is 0.847 gram per milliliter; the porocity is 0.980 gram per milliliter; and the calcium sulphate content reaches more than 99 percent, and all the parameters meet the standards of the pharmacopeia. The optimum processing technology for the gypsum also has the characteristic that the time from the room temperature to the calcining temperature of 650 DEG C is 50 minutes.
Description
Technical field
The present invention relates to a kind of technology for calcining method of gypsum, belong to the field of Chinese medicines.
Background technology
Gypsum is a Sulfates mineral anhydrite family gypsum, is " the tcm clinical practice medicine commonly used that Chinese pharmacopoeia is recorded.The plaster stone main component is CaSO
42H
2O.Beginning is stated from Shennong's Herbal and classifies middle product as.Flavor is hot, sweet.Property Great Cold.Attach to the lung and stomach meridians.Main effect is that heat-clearing and fire-purging, relieving restlessness are quenched the thirst.Be used for fever caused by exogenous pathogenic factors, high hot polydipsia, dyspnea and cough due to lung-heat, the high Sheng of stomach fire, headache, toothache.Forge then sweet, hot, puckery, cold.Attach to the lung and stomach meridians.Main effect is hygroscopic, myogenic, hold back sore, hemostasis.Control ulcer being unable to heal outward, eczema itch, burn due to hot liquid or fire, traumatic hemorrhage.Main component is CaSO
4
The concocting method of gypsum is with a long history, promptly forge that system, water fly ancient times, frying, vinegar system, simmer make, fire, multiple concocting method such as cannon." middle regulation of Chinese pharmacopoeia version in 2005 is forged gypsum to crisp according to method of direct calcination.Method of direct calcination is: get clean gypsum and put on the smokeless stove fire or put and forge in the suitable container to crisp or when being popular in, take out, cool and pulverize." national Chinese medicine preparation standard " (version in 1988) is slightly different, for: get clean plaster block and put in smokeless stove fire or the suitable container, heating is forged to little red with high heat, takes out, and cool back is fine ground." Shanghai City prepared slices of Chinese crude drugs concocted specification " (version in 1980) is honey system: get clean gypsum fritter, stir with refined honey 12%, fry to honeydew and be evenly distributed." Yunnan Province's prepared slices of Chinese crude drugs concocted specification " (version in 1986) forged for reverberatory furnace: get bulk drug and remove the silt particle be mingled with, often stir when putting into reverberatory furnace and forging, to all saturating hearts of medicine, taking-ups, canescence is given birth on dry in the air cold, surface, section is the strand shape, tarnish, and the time spent smashs to pieces." Zhejiang Province's Chinese medicine preparation standard " (version in 1986) urine soaks gypsum and is: the gypsum of rejecting when getting the system depositum urinae praeparatum, rinse, and drying is forged to being popular in, takes out, spreading for cooling, porphyrize is crossed 100 mesh sieves.
The main stream approach of the gypsum process of preparing Chinese medicine at present is the method for direct calcination of stipulating in the pharmacopeia, all there is not clearly regulation but thickness etc. is put in the time of calcining gypsum, temperature, granularity, shop up to now, the index of estimating technology for calcining all is the discriminating with sense organ, so be badly in need of finding out best processing procedure condition and evaluation index, be convenient to instruct and produce, increase the benefit
Summary of the invention
The objective of the invention is to overcome calcining gypsum technology in the market and do not have the clearly shortcoming of regulation forging system time, temperature, granularity, bedding thickness, thereby the technology for calcining of unified gypsum is provided, solve to produce take a lot of work, time-consuming, quality is uneven and be unfavorable for the problem of scale operation;
Another object of the present invention is to overcome the shortcoming of on the market gypsum quality of the system of forging only being differentiated with sense organ, provides with relative hardness, relative density, sedimentation, percentage of water loss and CaSO
4Content is the quality that index evaluation is forged the system gypsum.
The objective of the invention is to realize by following technical scheme:
A kind of processing method of calcining gypsum, step is as follows:
(1) terra alba is broken into 0.1～2cm
3Fritter, place crucible;
(2) select L18 (3
7) orthogonal table, select grinding particle size 0.125～0.5cm
3, forge 450～650 ℃ of temperature of system, forge system time 0.5～1.5h and bedding thickness 1～4cm as the investigation factor, each factor is respectively got 3 levels, by orthogonal table gypsum is forged system;
(3) the above-mentioned gypsum of forging system is measured relative hardness, relative density, sedimentation, percentage of water loss and CaSO respectively
4Content is investigated the quality of plaster of paris as index;
(4) result that step (3) is measured carries out score calculating respectively, draws comprehensive grading respectively;
(5) step (4) comprehensive grading result is carried out variance analysis, the optimization processing condition that draw calcining gypsum are that granularity is 0.125cm
3, forging the system temperature is 650 ℃, and forging the system time is 1.5h, and bedding thickness is 1cm;
(6) select temperature rise rate 20min～50min as single factor of investigating again, the gypsum of forging system through single factor is by measuring relative hardness, relative density, sedimentation, percentage of water loss and CaSO
4Content is investigated the quality of plaster of paris as index;
(7) the monofactorial measurement result of step (6) is carried out score respectively and calculate, draw comprehensive grading respectively;
(8) step (7) comprehensive grading result is carried out variance analysis, the temperature rise rate that draws calcining gypsum is that 650 ℃ of system temperature are forged in 50min arrival.
Investigation factor described in the above-mentioned steps (2) is respectively got 3 levels, is respectively grinding particle size 0.125cm
3, 0.25cm
3, 0.5cm
3, forge 450 ℃, 550 ℃, 650 ℃ of system temperature, forge system time 0.5h, 1h, 1.5h, bedding thickness 1cm, 2cm, 4cm.
Comprehensive product described in above-mentioned steps (4), (7) are divided into: comprehensive grading=relative hardness score * 0.1+ relative density score * 0.2+ sedimentation score * 0.2+ percentage of water loss * 0.2 score C aCO
3Content score * 0.3.
Thereby the technology for calcining of determining gypsum the best is 0.125cm for being ground into granularity
3Fritter, bedding thickness is 1cm, is warming up in 50 minutes to forge 650 ℃ of system temperature, forging the system time is 1.5h.
Beneficial effect of the present invention:
The invention provides with grinding particle size, forge the system temperature, forge system time and bedding thickness and temperature rise rate and unify the technology of calcining gypsum as the investigation factor; Also proposed with relative hardness, relative density, sedimentation, percentage of water loss and CaSO simultaneously
4Content does not have unified calcining gypsum technology as the quality of index investigation plaster of paris for a long time thereby solved, and investigates the problem that the plaster of paris quality does not have clear and definite investigation index, has solved the inhomogenous problem of quality for a long time of producing yet.
Embodiment
Embodiment 1, the technological experiment of calcining gypsum
1. laboratory apparatus:
Retort furnace, Shanghai Precision Scientific Apparatus Co., Ltd, SX2-4-10 type;
Analytical balance, Shanghai Precision Scientific Apparatus Co., Ltd, HANK-PN FA1104N.
2. experimental technique:
2.1 L18 (3 is selected in experiment for use
7) the orthogonal table design, with the gypsum granularity, forge the system temperature, forge the system time, the container middle berth is put thickness as the investigation factor, each factor is respectively selected three levels (seeing Table 1).
Table 1: processing procedure level of factor table
2.1.1 observation index:
It is crisp only to have stipulated to forge system in the pharmacopeia, and this is the judgement of a sense organ, judges the quality of calcining product accurately for science more, and we are in conjunction with hardness, percentage of water loss, relative density, sedimentation and CaSO
4Five indexs of content are investigated technology for calcining, set up the objective appraisal standard.
Hardness: hardness is meant that mineral resist the ability of external mechanical effect, it is one of important evidence of mineral, because slick plane can not appear in sample in testing, and therefore can't adopt hardness tester to measure accurate hardness, and adopts the relative hardness after the mohs hardness meter is determined the sample process of preparing Chinese medicine.Method is to select the sharp-pointed position of plaster of paris, on the formula of the rubbing sclerometer of known hardness, delineate, the test of scratch hardness is carried out from low to high successively, observe the sclerometer plane no marking is arranged, have cut then sample hardness greater than sclerometer, no marking sample hardness is less than sclerometer, and the more higher leveled sclerometer of test successively again is until between between two hardness ranks or till the quite a certain sclerometer.
Percentage of water loss: according to every experiment number accurately claim the weight before and after the system of forging, calculate percentage of water loss.
Relative density: relative density is an important physical constant of material, the accurate earlier sample that claims to decide certainweight during mensuration, during mensuration sample is put into the graduated cylinder that certain volume water is housed, the volume of liter waterborne is sample volume, calculates the relative density of sample according to quality and volumeter.
Sedimentation: sedimentation is the quality of unit volume fine powder (100 order), example pharmaceuticals is broken into fine powder cross 100 mesh sieves, fine powder after will sieving again piles with the container (weighing bottle of constant weight) of a known volume naturally, scrape off the fine powder that exceeds bottleneck with cutter, the quality that fine powder decided in tight title, dg=m/V tries to achieve sedimentation according to formula.
CaSO
4Content: each experiment is carried out assay by current edition pharmacopeia " plaster of paris " time content assaying method to it number after the system of forging.Concrete grammar is for getting the about 0.2g of plaster of paris fine powder, the accurate title, decide, and puts in the Erlenmeyer flask, adds dilute hydrochloric acid 10ml, heating for dissolving, add 1 of water 100ml and methyl red indicating liquid, drip potassium hydroxide test solution to solution and show light yellow, continue to add 5ml again, it is a small amount of to add the fluorexon indicator, with Calcium Disodium Versenate (0.05mol/L) titration,, and show orange to the yellow-green fluorescence disappearance of solution.Every 1ml Calcium Disodium Versenate (0.05mol/L) is equivalent to the hydrous calcium sulfate (CaSO of 8.608mg
42H
2O)
2.1.2 experimental result:
Orthogonal experiments is analyzed
Each organizes to such an extent that be divided into Y/Y
All
Total score=0.1Y1+0.2Y2+0.2Y3+0.2Y4+0.3Y5
Variance analysis
**F0.01(2，6)＝10.92
*F0.05(2，6)＝5.14
**p<0.01
*p<0.05
According to last analysis, optimum process condition is A
1B
3C
3D
1
2.1.3 confirmatory experiment
Each observation index of plaster of paris under the optimised process
2.2 on the basis of optimised process, investigate of the influence of temperature rise rate list factor, promptly investigate by room temperature and rise to the influence of the time of temperature required (650 ℃) to calcining gypsum to calcining gypsum.
2.2.1 the same 2.1.1 of observation index
2.2.2 experimental result
The interpretation of result of temperature rise rate list factor
Each organizes to such an extent that be divided into Y/Y
All
Total score=0.1Y1+0.2Y2+0.2Y3+0.2Y4+0.3Y5
One-way analysis of variance
3. discuss
Chemical transformation has not only taken place before and after the calcining gypsum, variation has also taken place in its physical property, this experiment changes in the past only with the limitation of chemical ingredients as the processing procedure screening index, adopt fast, accurately, sensitivity intuitively physico-chemical process to plaster of paris hardness, percentage of water loss, relative density, sedimentation and CaSO
4Five indexs of content are investigated technology for calcining.
Learnt that by orthogonal experiments the key factor that influences the gypsum concocted quality is to forge the system temperature and forge the system time, its optimum process condition is B
3And C
3, i.e. 650 ℃ and 1.5h, secondly influence factor is a grinding particle size, its optimum process condition is A
1, i.e. 0.125cm
3And it is less to the processing procedure influence to put thickness at the container middle berth, can get convenient operation by enterprise condition and get final product.Thereby reach a conclusion, the optimum technology for calcining of gypsum should be and is ground into granularity is 0.125cm
3Fritter, spread to 1cm thick, under 650 ℃, forge the system 1.5 hours.
Press A
1B
3C
3D
1Carry out proof test, 3 parts of plaster of paris of gained are loose, crisp, and average percentage of water loss is 20.83%; Average relative density is 0.847g/ml, and sedimentation is 0.980g/ml, and its calcium sulphate content has reached more than 99%, and good reproducibility meets standards of pharmacopoeia.
Investigate the result by temperature rise rate list factor and learn, slowly be warming up to the best and forge the system temperature, the arrival assigned temperature was better to the system of the forging effect of gypsum in promptly 50 minutes.
Therefore reach a conclusion, calcining gypsum technology is for being ground into 0.125cm
3Fritter, spread to 1cm, rose to 650 ℃ by room temperature in 50 minutes after the system of forging 1.5 hours.
Claims (3)
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|---|---|---|---|
| CNA2008102433026A CN101439940A (en) | 2008-12-26 | 2008-12-26 | Technological process for calcining gypsum |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| Publication Number | Publication Date |
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| CN101439940A true CN101439940A (en) | 2009-05-27 |
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ID=40724574
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106176802A (en) * | 2016-07-18 | 2016-12-07 | 北京中医药大学 | A kind of Gypsum Fibrosum concocting method |
-
2008
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106176802A (en) * | 2016-07-18 | 2016-12-07 | 北京中医药大学 | A kind of Gypsum Fibrosum concocting method |
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Open date: 20090527 |