CN1563934A - Small spray drying appts. for lab and its application method - Google Patents
Small spray drying appts. for lab and its application method Download PDFInfo
- Publication number
- CN1563934A CN1563934A CN 200410017927 CN200410017927A CN1563934A CN 1563934 A CN1563934 A CN 1563934A CN 200410017927 CN200410017927 CN 200410017927 CN 200410017927 A CN200410017927 A CN 200410017927A CN 1563934 A CN1563934 A CN 1563934A
- Authority
- CN
- China
- Prior art keywords
- sample
- hothouse
- spray
- sample bottle
- drying
- 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.)
- Granted
Links
- 238000001694 spray drying Methods 0.000 title claims description 21
- 238000000034 method Methods 0.000 title claims description 5
- 239000007921 spray Substances 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 18
- 238000005507 spraying Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 9
- 238000009434 installation Methods 0.000 claims description 10
- 239000004927 clay Substances 0.000 claims description 9
- 238000011084 recovery Methods 0.000 claims description 9
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 8
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 8
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000000889 atomisation Methods 0.000 claims description 3
- 239000002518 antifoaming agent Substances 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 229910021647 smectite Inorganic materials 0.000 claims description 2
- 238000010276 construction Methods 0.000 claims 1
- 239000000725 suspension Substances 0.000 claims 1
- 239000007787 solid Substances 0.000 abstract description 3
- 238000005485 electric heating Methods 0.000 abstract 1
- 239000008187 granular material Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 8
- 238000000227 grinding Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 101100342486 Oryza sativa subsp. japonica KSL10 gene Proteins 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- HGAZMNJKRQFZKS-UHFFFAOYSA-N chloroethene;ethenyl acetate Chemical compound ClC=C.CC(=O)OC=C HGAZMNJKRQFZKS-UHFFFAOYSA-N 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
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- Drying Of Solid Materials (AREA)
Abstract
Spray gun of sprayer unit is connected to sample bottle in small volume and compressed air line. Drying unit includes a columnar drying chamber, a dismountable coniform cover with a hole in top, and electric heating tube connected to temperature control sensor in bottom. Solid powder is dispersed on solution of polyvinyl alcohol in solid to liquid ratio as 1:1.5-1.2.5, and spraying pressure 0.70-1.10kg/cm2 and drying temperature 100-150 deg.C. Dried 10-50 micro spherical granules powder possesses good rheological behavior. The invention is applicable to a small quantity of powder used in lab.
Description
Technical field
The invention belongs to the powder handling technology, relate in particular to the spray drying of powder.
Background technology
The spray-drying installation of powder is widely used in the preparation of breeze, inorganic powdered material, medicine, biomaterial.It generally includes spraying and dry two parts system and device.In the market, this device volume is bigger, reaches several cubic meters, the structure heaviness, and the recovery of sample is low, and it can only be used for the bigger place of sample size requirement.But under laboratory condition, generally need spray-dired sample size less or sample source is few, quantitative and the qualitative analysis as the X-ray diffraction of mineral, often require sample not have preferred orientation, the spray drying treatment sample is best processing mode, but the demand to sample is few, have 1～5 gram sample just enough, this reaches spray-dired requirement with regard to being difficult to commercially available spraying apparatus; In addition, when the powder body material test of high rheological, also require the small sample spray drying.
Summary of the invention
The present invention seeks to solve the problem that prior art exists, the laboratory that a kind of compact conformation is provided is with small-sized spraying plant and using method thereof.
For achieving the above object, this spray-drying installation technical scheme comprises spraying and dry two parts device.Its architectural feature is sample bottle and the compressed air piping that the spray gun of spraying plant connects little volume; Drum shape hothouse is arranged in drying device, conical top cover is arranged above it, the hole is established in top cover upper end, between hothouse cylinder body and the top cover for removably connecting; In the hothouse bottom electrothermal tube is housed, electrothermal tube and temperature controller and temperaturecontrol sensor link.
The using method of above-mentioned spray-drying installation is as follows:
One, supending
Earlier be that 30000～70000 tygon 0.5 gram is dissolved in the 100mL ethanolic solution with molecular weight, produce concentration and be 0.5% poly-vinyl alcohol solution,＜200 purpose solid powders are scattered in the poly-vinyl alcohol solution again, poly-vinyl alcohol solution plays the effect of bonding agent.For the sample of high clay content, have good cohesive equally with clear water (without poly-vinyl alcohol solution), add 1 antifoaming agent n-octyl alcohol solution (1-octanol (CH
3(CH
2)
7OH) be dissolved in alcohol) foaming phenomenon in the time of can avoiding disperseing.
The amount of powder and poly-vinyl alcohol solution consumption in the suspending liquid (being the solid-liquid ratio) depend on the character of sample.For non-clay class powder, 1: 1.5～1: 2.5 commonly used.General solid-liquid ratio is can both obtain preferably effect at 1: 2.For some clay, solid-liquid is bigger than changing, and as the smectite clay, can reach 1: 6, can produce the suspending liquid of appropriate flow sex change by further dilution.
The suitable suspending liquid of preparation concentration is the key that the spraying sample is prepared.Higher solid-liquid is than the spherical-like morphology that can reduce drying time and assurance dried particles; And lower solid-liquid ratio is easier to pass through nozzle and nonchoking nozzle under low-pressure.Experiment shows, considers the recovery of product, and best atomisation pressure is 0.70～1.10kg/cm
2Pressure is high more, and drop is thin more, and the spheric grain of product is more little.In fact, the product particle diameter can cause in its thermal current that is suspended in hothouse during less than 10 μ m, and can not be deposited in the bottom of hothouse; Lower spray gun pressure, the drop spouting velocity is slower, and is longer with the duration of contact of thermal current, bone dry in the time of at the bottom of dropping to case.The viscosity of suspending liquid has also influenced the size of ejection droplet.Viscosity is big, and droplet is big, but difficult ejection under the low pressure.
Two, the operation steps of spray-drying installation
1, dry kiln.Start electrothermal tube, by monitoring of the temperature control sensor in the hothouse addendum cone and control temperature.Heat and can reach 150 ℃ in 10～15 minutes, at this moment the temperature of hothouse body bottom is about 90 ℃.
For general sample, the temperature in the hothouse is controlled at 100～150 ℃ and can both meets the demands.Temperature is too low, can make sample fully drying just fall at the bottom of the hothouse;
2, after reaching predetermined temperature, a sizeable paper places the bottom of hothouse, is used to hold the sample after the spray drying.Deployed suspending liquid is moved into the spray gun sample bottle, and connect with the spray gun interface thread.Regulate tensimeter pressure to 0.70～1.10kg/cm
2Then, pistol, vertical downwards in hothouse vertex of a cone mouth, the manual Switch of spray pistol size of regulating sprays into suspending liquid in the hothouse with the control flow velocity.Simultaneously, shaking sample bottle gently makes the suspending liquid in it even.Whole suspending liquid can be sprayed into hothouse in about 1～5 minute;
3, pull out the paper of containing sample gently, collect the dry sample on it standby;
4, cleaning sample bottle and spray gun.Clear water is filled sample bottle, regulate pressure to 3kg/cm
2, open the gun controls switch, spraying is cleaned, three times repeatedly.Changing another sample or preservation again treats to use next time.
Three, the recovery of dry sample
Typical spray drying sample presents the spheric grain of diameter 10～50 μ m.The weight of original powder sample weight of weighing and dry powder sample can calculate the dried recovered rate.General dried recovered rate can reach 80～85%.
Elevated pressures is (as 1.10kg/cm
2) under spray drying, often, be easy to be suspended in the hot-air or float in the air because droplet is thinner, and the spheric grain of dry sample is also less, the recovery at this moment is then lower, sometimes only 50%.Lower pressure is (as 0.70kg/cm
2) under spray drying, the recovery can reach more than 80%.
Advantage of the present invention, owing to adopt the airbrush (spray gun) of drawing usefulness and the hothouse of little volume, compact conformation, the required powder sample amount of spraying sample is few, the hothouse of small sample bottle and corresponding volume, the sample size of required powder is few, is specially adapted to the laboratory and uses, and the powder rheological that obtains after the spray drying is good; And drying device is convenient to clean.
Description of drawings
Fig. 1 is the structural representation of spray-drying installation of the present invention.
Embodiment
With reference to the description of drawings embodiment:
As shown in the figure, air compressor machine 13 compressed air ducts 4 link to each other with spray gun 1 in the spraying plant, be connected the front of gun controls switch 2, there is small sample bottle 3 to be connected with spray gun 1 in the back of gauge tap. sample bottle, compressed air hose pipeline joint and spray gun constitute one, the Crescendo No 175-7 airbrush that can adopt commercial airbrush BadgerAir-Brush Co made in U.S.A to produce, the sample bottle that it is 20mL that this airbrush (spray gun) carries a volume, bottleneck links to each other with screw thread with spray gun; The compressed air hose pipeline joint is arranged on spray gun, and pressurized air can produce the air capacity 0.08M of this air compressor machine by KS10 type air compressor machine 13
3/ min, top pressure 0.8MPa, power of motor 0.75kw is enough to provide required pressurized air.
Drying device mainly is a hothouse 5, it makes the drum body of φ 40cm * 85cm by the thick aluminium sheet of 2mm, and the 1000W electrothermal tube 7 of 2 parallel connections is housed in its bottom, is around on wide one section of drum bottom 15cm, and be fixed on the cylinder body, its outside is incubated with insulation materials such as asbestos cloth parcel.Electrothermal tube connects with electronic temperature controller 8, temperature control sensor 9 (temperature thermocouple).The bottom half of hothouse adds the footing 10 of two wide 5cm of long 20cm, and makes the hothouse casing be higher than footing bottom surface 0.5cm.The cone angle that the top cover of hothouse body is made by the 2mm aluminium sheet is 90 ° a cone 6, and the vertex of a cone is clipped and kept the hole that a diameter is 2.5cm, for spraying 12 usefulness.Be detachable between the vertex of a cone of hothouse and the drum body and connect, be convenient to clean.
Use the present invention to the spray-dired embodiment of sample:
Take by weighing＜200 purpose kaolinite clay, 6.2 grams, adding concentration is 0.5% poly-vinyl alcohol solution 15mL, fully stirring or put into miniature grinding machine grinding fully was mixed it in 3 minutes, and make suspending liquid, move in the sample bottle 3 of spray gun, can add 1～2mL clear water and clean grinding machine, for improving the recovery, cleaning fluid also moves in the sample bottle.
Dry kiln makes it reach 120 ℃.The paper 11 of placing 38 * 50cm size is in the drying box bottom.The adjusting atomisation pressure is 0.70kg/cm
2Pistol makes the vertical sensing hothouse of nozzle in hothouse bellmouth top, opens Switch of spray pistol gently, finishes the spray drying of smalite sample in 2 minutes.
Extract the paper 11 of containing sample out, collect dry sample.Cross and claim to such an extent that dry sample 5.5 restrains.The recovery is 5.2/6.2=84%.
Last cleaning spray gun and sample bottle.
Dry sample is tiled in the specimen holder of X-ray diffraction analysis usefulness, makes omnidirectional sample.With the XRD figure spectrum that it obtains, good reproducibility, no preferred orientation is suitable for quantitative examination.
Claims (6)
1, the small-sized spray-drying installation used of a kind of laboratory comprises spraying and dry two parts device, it is characterized in that the sample bottle (3) and the compressed air piping (4) of the little volume of spray gun (1) connection of spraying plant; Drum shape hothouse (5) is arranged in drying device, conical top cover (6) is arranged above it, and the hole is established in top cover upper end, between hothouse cylinder body and the top cover for removably connecting, electrothermal tube (7) is housed in the hothouse bottom, and electrothermal tube and temperature controller (8) and temperaturecontrol sensor (9) link.
2, by the described small-sized spray-drying installation of claim 1, it is characterized in that spray gun (1) and sample bottle (3) and compressed air hose pipeline joint are one-piece construction, adopt Crescendo 175-7 type airbrush.
3, the using method of the small-sized spray-drying installation used of laboratory according to claim 1 is characterized in that operation steps is as follows:
One, supending
With＜200 purpose pressed powders be scattered in that molecular weight is 30000～70000, concentration is in 0.5% the poly-vinyl alcohol solution.For the sample of high clay content, then it is scattered in the clear water, add 1 antifoaming agent n-octyl alcohol solution; Solid-to-liquid ratio in the suspending liquid between the amount of powder and the poly-vinyl alcohol solution consumption depends on the character of sample, for non-clay class powder, gets 1: 1.5～1: 2.5, and for some clay class, as the smectite clay, the solid-liquid ratio can reach 1: 6;
Two, the use step of spray-drying installation
1, dry kiln (5) starts electrothermal tube (7) by monitoring of the temperature control sensor (9) in the hothouse addendum cone (6) and control temperature, heats 10～15 minutes, and the temperature in the hothouse is controlled at 100～150 ℃;
2, after reaching predetermined temperature, a sizeable paper (11) is placed the bottom of hothouse, deployed suspending liquid is moved into spray gun sample bottle (3), the control atomisation pressure is 0.70～1.10kg/cm
2Then, pistol, vertical downwards in hothouse vertex of a cone mouth, manual size of regulating Switch of spray pistol sprays into sample bottle inner suspension liquid in the hothouse, with the control flow velocity simultaneously, shake sample bottle gently and make the suspending liquid in it even, whole suspending liquid were sprayed into hothouse in about 1～5 minute;
3, pull out the paper (11) of containing sample gently, collect the dry sample on it standby;
4, cleaning sample bottle (3) and spray gun (1) are filled sample bottle with clear water, regulate pressure to 3kg/cm
2, open the gun controls switch, spraying is cleaned, and three times repeatedly, changes another sample or preservation again and treats to use next time;
Three, the recovery of dry sample
The recovery sample diameter is the spheric grain of 10～50 μ m after the spray drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100179272A CN100395535C (en) | 2004-04-21 | 2004-04-21 | Small spray drying appts. for lab and its application method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100179272A CN100395535C (en) | 2004-04-21 | 2004-04-21 | Small spray drying appts. for lab and its application method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1563934A true CN1563934A (en) | 2005-01-12 |
| CN100395535C CN100395535C (en) | 2008-06-18 |
Family
ID=34479237
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100179272A Expired - Fee Related CN100395535C (en) | 2004-04-21 | 2004-04-21 | Small spray drying appts. for lab and its application method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100395535C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103460052A (en) * | 2011-02-25 | 2013-12-18 | 通用电气医疗集团英国有限公司 | Paper support and method of recovering biological material therefrom |
| CN104436723A (en) * | 2014-12-02 | 2015-03-25 | 四川绵竹川润化工有限公司 | Integrated drying and pneumatic crushing process |
| CN110018281A (en) * | 2019-05-20 | 2019-07-16 | 华核（天津）新技术开发有限公司 | Radioactive decontamination efficiency test device |
| CN110496410A (en) * | 2019-09-09 | 2019-11-26 | 湖北金晟远环保科技股份有限公司 | A kind of polyaluminium chloride drum-type drying equipment |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2651825A1 (en) * | 1976-11-13 | 1978-05-18 | Bayer Ag | IMPROVED SIGHTING IN THE SPRAY TOWER |
| CN2200167Y (en) * | 1994-05-20 | 1995-06-07 | 华忆陶磁原料股份有限公司 | Feldspar powder spraying drying machine |
| CN1202989C (en) * | 2002-05-09 | 2005-05-25 | 四川龙蟒集团有限责任公司 | Process for concentrating diluted sulfuric acid and removing impurities |
| DE10241447A1 (en) * | 2002-09-06 | 2004-03-18 | Rähse, Wilfried, Dr. | Flash-drying ultra-fine dry powder comprising mixture of ingredients involves using specific temperature and pressure conditions |
| CN2699969Y (en) * | 2004-04-21 | 2005-05-18 | 浙江大学 | Minitype spray drying device for laboratry |
-
2004
- 2004-04-21 CN CNB2004100179272A patent/CN100395535C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103460052A (en) * | 2011-02-25 | 2013-12-18 | 通用电气医疗集团英国有限公司 | Paper support and method of recovering biological material therefrom |
| CN104436723A (en) * | 2014-12-02 | 2015-03-25 | 四川绵竹川润化工有限公司 | Integrated drying and pneumatic crushing process |
| CN104436723B (en) * | 2014-12-02 | 2016-05-04 | 四川绵竹川润化工有限公司 | A kind of dry gentle powder integral process |
| CN110018281A (en) * | 2019-05-20 | 2019-07-16 | 华核（天津）新技术开发有限公司 | Radioactive decontamination efficiency test device |
| CN110496410A (en) * | 2019-09-09 | 2019-11-26 | 湖北金晟远环保科技股份有限公司 | A kind of polyaluminium chloride drum-type drying equipment |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100395535C (en) | 2008-06-18 |
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Granted publication date: 20080618 Termination date: 20100421 |