CN111822106A - Method for preparing superfine pear stone cell powder - Google Patents

Method for preparing superfine pear stone cell powder Download PDF

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Publication number
CN111822106A
CN111822106A CN202010597327.7A CN202010597327A CN111822106A CN 111822106 A CN111822106 A CN 111822106A CN 202010597327 A CN202010597327 A CN 202010597327A CN 111822106 A CN111822106 A CN 111822106A
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China
Prior art keywords
stone cell
pear stone
pear
powder
cell powder
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CN202010597327.7A
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Chinese (zh)
Inventor
杨勇
朱泽慧
孙雅雯
施晓琪
曹周
陈桂平
喻春皓
张孝杰
钱运华
杜卫刚
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Huaiyin Institute of Technology
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Huaiyin Institute of Technology
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Priority to CN202010597327.7A priority Critical patent/CN111822106A/en
Publication of CN111822106A publication Critical patent/CN111822106A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/04—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with unperforated container
    • B02C17/08—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with unperforated container with containers performing a planetary movement
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9789—Magnoliopsida [dicotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/99—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from microorganisms other than algae or fungi, e.g. protozoa or bacteria
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/18—Details
    • B02C17/183—Feeding or discharging devices
    • B02C17/186—Adding fluid, other than for crushing by fluid energy
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/84—Products or compounds obtained by lyophilisation, freeze-drying

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Birds (AREA)
  • Food Science & Technology (AREA)
  • Biotechnology (AREA)
  • Epidemiology (AREA)
  • Botany (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Tropical Medicine & Parasitology (AREA)
  • Crushing And Grinding (AREA)
  • Cosmetics (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a method for preparing superfine pear stone cell powder, which comprises the following steps: (1) placing the pear stone cell extraction particles into a plant crusher, and performing pre-crushing to prepare pear stone cell coarse powder; (2) adding the coarse pear stone cell powder, water, a dispersing agent and a defoaming agent into a planetary ball mill simultaneously for ball milling and crushing; (3) and (3) centrifuging, filtering and washing the suspension obtained in the step (2), and freeze-drying to obtain superfine pear stone cell powder. The invention prepares the superfine pear stone cell powder by wet method crushing in a planetary ball mill, and breaks the pear stone cell cluster particles to obtain particles which meet the requirement of particle size and have uniform size, and the particles are used for toothpaste abrasive without the problem of bioactive component release.

Description

Method for preparing superfine pear stone cell powder
Technical Field
The invention belongs to the technical field of natural biological material ultrafine grinding, and relates to a method for preparing ultrafine pear stone cell powder.
Background
The abrasive in the toothpaste can be matched with a toothbrush to wipe off tartar on the surface of teeth and reduce foreign matters such as tooth stain, dental calculus, dental plaque and the like. At present, all toothpaste abrasives are inorganic superfine materials, mainly calcium carbonate and hydrated silicon dioxide, and have the defects of high hardness, damage to teeth caused by long-term use, and harm to health particularly when infants swallow the toothpaste abrasives. The pear stone cells are hard dregs in pear fruits and exist in single grains or aggregated clusters in the fruits, and the size of the extracted pear stone cell clusters is about 10-150 microns. The main components of the pear stone cells are lignin and cellulose, have certain hardness and granularity, and can be used as an abrasive to be added into the children no-clean toothpaste. In order to ensure the safe, effective and comfortable mouthfeel of the toothpaste, the pear stone cell abrasive has proper particle diameter and uniform size, and the particle diameter is required to be 1-50 microns.
The existing method for preparing superfine powder of bio-based material aims to break plant cell walls and release internal active ingredients as much as possible. Zhang Min adopts high-energy nanometer impact mill to crush naked oat bran coarse powder into particles of 0.4 micron. Ultrafine grinding the freeze-dried rose by using a bidirectional rotary ball mill to obtain rose powder with median particle size of 6.1 microns. These methods are costly, complex processes, and have high requirements for controlling equipment and production process conditions.
Disclosure of Invention
Aiming at the problems of overlarge particle size and nonuniform particle size of the pear stone cell particles in the prior art, the invention aims to provide a method for preparing superfine pear stone cell powder, the superfine pear stone cell powder is prepared by wet grinding in a planetary ball mill, and the pear stone cell cluster particles are crushed to obtain particles which meet the particle size requirement and are uniform in size, the particles are used for a toothpaste friction agent, and the problem of release of bioactive components does not exist.
The invention is realized by the following technical scheme:
a method for preparing superfine pear stone cell powder comprises the following steps:
(1) placing the pear stone cell extraction particles into a plant crusher, and performing pre-crushing to prepare pear stone cell coarse powder;
(2) adding the coarse pear stone cell powder, water, a dispersing agent and a defoaming agent into a planetary ball mill simultaneously for ball milling and crushing;
(3) and (3) centrifuging, filtering and washing the suspension obtained in the step (2), and freeze-drying to obtain superfine pear stone cell powder.
The invention further improves the scheme as follows:
in the step (1), the pre-crushed pear stone cell coarse powder needs to be sieved by a 30-120-mesh sieve, and preferably sieved by a 100-mesh sieve.
In the step (2), the mass ratio of the water, the dispersing agent and the defoaming agent is 1: 0.2-1 ‰, and preferably 1:0.5 ‰, 0.5 ‰.
In the step (2), the mass ratio of the feed liquid is 1: 4-10, preferably 1: 6.
The planetary ball mill is a unidirectional rotary ball mill, and a grinding medium in the ball mill is ceramic beads, glass beads, zirconia beads or quartz sand with the diameter of 1-10 mm, preferably zirconia beads with the diameter of 2 mm.
Wherein the mass ratio of the pellets is 1: 1-4, preferably 1:2, and the filling coefficient is 30-60%, preferably 40%.
The ball milling and crushing time of the planetary ball mill is 60-240 minutes, preferably 120 minutes, the ball milling and crushing temperature is 20-70 ℃, the ball milling and crushing temperature is preferably 30 ℃, the rotating speed is 200-600 revolutions per minute, and preferably 400 revolutions per minute.
The defoaming agent is sodium methylene dinaphthalene sulfonate or sodium lignin sulfonate or a mixture of the sodium methylene dinaphthalene sulfonate and the sodium lignin sulfonate. The defoaming agent is organosilicon defoaming agent S2100 or tributyl phosphate or a mixture of the two.
In the step (3), when the suspension is centrifuged, the rotating speed of a centrifuge is 4000-6000 rpm, the washing is water washing, ethanol washing and water washing in sequence, and the temperature of freeze drying is-15 to-30oC. The time is 8-14 h.
The material-liquid ratio is as follows: the ratio of the mass of the pear stone cell powder to the mass of water.
The material ball mass ratio is as follows: the ratio of the total mass of the pear stone cells, water, defoamer and dispersant to the mass of the grinding medium.
The filling factor is as follows: the ratio of the material contained in the star ball mill to the total volume of the vessel.
The invention has the beneficial effects that:
the invention prepares superfine pear stone cell powder by wet grinding in a planetary ball mill, and breaks the pear stone cell cluster particles to obtain particles which meet the particle size requirement and have uniform size, and the median particle size D of the superfine pear stone cell powder50Reaching 40 microns, is used for toothpaste abradant, and has no problem of bioactive component release.
The method provided by the invention has the characteristics of high processing modernization degree, simple operation and large treatment capacity, can realize continuous production, has high safety performance, is beneficial to industrialization, and is a novel method suitable for large-scale industrial preparation of ultrafine pear stone cell powder.
Drawings
FIG. 1 is a microscopic view of the extracted granule from pear stone cells before pulverization;
FIG. 2 is a microscopic view of the ultrafine pear stone cell powder after pulverization of example 1;
FIG. 3 is a graph showing a distribution of particle sizes of ultrafine pear stone cell powders after pulverization in example 1;
as can be seen from FIG. 1, the extracted pear stone cells are aggregated clusters of single pear stone cells, and the particle size is about 200 microns.
As can be seen from figure 2, the wet-ground pear stone cells exist as single particles, the particle size is 20-40 microns, the appearance is complete, and the pear stone cells are regular spherical particles.
Fig. 3 is a particle size distribution of the pear stone cell powder measured by a malvern laser particle size analyzer, wherein it can be seen that the particle size of the pear stone cell powder after wet grinding is mainly 20-40 micrometers, and the particle size is uniform.
Detailed Description
Example 1
The wet crushing method for preparing superfine pear stone cell powder in a planetary ball mill comprises the following steps:
(1) placing the pear stone cell extraction particles into a plant pulverizer, performing pre-pulverization to prepare pear stone cell coarse powder, and sieving the obtained coarse powder with a 100-mesh sieve.
(2) Adding the coarse pear stone cell powder, water, a dispersing agent and a defoaming agent into a planetary ball mill simultaneously for ball milling and crushing; the material-liquid ratio in the planetary ball mill is 1:6, the dispersant is sodium lignosulfonate with the dosage of 0.5 per mill of water, the defoamer is tributyl phosphate with the dosage of 0.5 per mill of water, the grinding medium is zirconia beads with the diameter of 2 millimeters, the rotating speed of the planetary ball mill is 400 r/min, the grinding temperature is 40 r/minoC, the mass ratio of the material balls is 1:2, the filling coefficient is 50%, and the grinding time is 120 minutes.
(3) Centrifuging the suspension obtained in the step (2), wherein the rotating speed of a centrifugal machine is 4000 revolutions per minute, the centrifuging time is 60 minutes, and the obtained solid is sequentially deionized water and waterWashing with ethanol for 1 time, and freeze drying at-15 deg.C overnight to obtain superfine pear stone cell powder; detecting the particle diameter D of the pear stone cell powder50Is 32 μm, D90Is 50 microns.
Example 2
The wet crushing method for preparing superfine pear stone cell powder in a planetary ball mill comprises the following steps:
(1) placing the pear stone cell extraction particles into a plant pulverizer, performing pre-pulverization to prepare pear stone cell coarse powder, and sieving the obtained coarse powder with a 30-mesh sieve.
(2) Adding the coarse pear stone cell powder, water, a dispersing agent and a defoaming agent into a planetary ball mill simultaneously for ball milling and crushing; the material-liquid ratio in the planetary ball mill is 1:4, the dispersant is sodium methylene dinaphthalenesulfonate, the dosage is 1 per mill of water, the defoamer is tributyl phosphate, the dosage is 1 per mill of water, the grinding medium is ceramic beads with the diameter of 10 millimeters, the rotating speed of the planetary ball mill is 200 r/min, the grinding temperature is 70 r/minoC, the mass ratio of the material balls is 1:1, the filling coefficient is 30%, and the grinding time is 60 minutes.
(3) And (3) centrifuging the suspension obtained in the step (2), washing the obtained solid for 1 time by using deionized water and ethanol sequentially at the rotating speed of a centrifuge of 6000 rpm for 60 minutes, and freeze-drying the solid overnight at the temperature of minus 30 ℃ to obtain the ultrafine pear stone cell powder. Detecting the particle diameter D of the pear stone cell powder50Is 29 μm, D90Is 65 microns.
Example 3
The wet crushing method for preparing superfine pear stone cell powder in a planetary ball mill comprises the following steps:
(1) placing the pear stone cell extraction particles into a plant pulverizer, performing pre-pulverization to prepare pear stone cell coarse powder, and sieving the obtained coarse powder with a 120-mesh sieve.
(2) Adding the coarse pear stone cell powder, water, a dispersing agent and a defoaming agent into a planetary ball mill simultaneously for ball milling and crushing; the material-liquid ratio in the planetary ball mill is 1:10, the dispersant is sodium methylene dinaphthalenesulfonate, the dosage is 1 per mill of water, the defoamer is tributyl phosphate, the dosage is 1 per mill of water, the grinding medium is zirconia beads with the diameter, and the planetary ball mill is characterized in thatThe rotation speed of the ball mill is 600 revolutions per minute, and the grinding temperature is 20oC, the mass ratio of the material balls is 1:4, the filling coefficient is 60 percent, and the grinding time is 240 minutes.
(3) And (3) centrifuging the suspension obtained in the step (2), washing the obtained solid for 1 time by using deionized water and ethanol sequentially at the rotating speed of a centrifuge of 6000 rpm for 60 minutes, and freeze-drying the solid overnight at the temperature of minus 30 ℃ to obtain the ultrafine pear stone cell powder. Detecting the particle diameter D of the pear stone cell powder50Is 31 μm, D90Is 59 microns.

Claims (9)

1. A method for preparing ultrafine pear stone cell powder is characterized by comprising the following steps:
(1) placing the pear stone cell extraction particles into a plant crusher, and performing pre-crushing to prepare pear stone cell coarse powder;
(2) adding the coarse pear stone cell powder, water, a dispersing agent and a defoaming agent into a planetary ball mill simultaneously for ball milling and crushing;
(3) and (3) centrifuging, filtering and washing the suspension obtained in the step (2), and freeze-drying to obtain superfine pear stone cell powder.
2. The method of claim 1, wherein the ultrafine pear stone cell powder is prepared by: in the step (1), the pre-crushed pear stone cell coarse powder needs to be sieved by a 30-120-mesh sieve.
3. The method of claim 1, wherein the ultrafine pear stone cell powder is prepared by: in the step (2), the mass ratio of the water to the dispersant to the defoaming agent is 1: 0.2-1 ‰: 0.2-1 per mill, and the mass ratio of the feed liquid is 1: 6-10.
4. The method of claim 1, wherein the ultrafine pear stone cell powder is prepared by: in the step (2), the planetary ball mill is a unidirectional rotary ball mill, and a grinding medium in the ball mill is ceramic beads, glass beads, zirconia beads or quartz sand with the diameter of 2-10 mm.
5. The method for preparing ultrafine pear stone cell powder according to any one of claims 1, 3 or 4, wherein: in the step (2), the mass ratio of the material balls is 1: 1-4, and the filling coefficient is 30-60%.
6. The method for preparing ultrafine pear stone cell powder according to any one of claims 1 or 3, wherein: in the step (2), the defoaming agent is sodium methylene dinaphthalene sulfonate or sodium lignin sulfonate or a mixture of the sodium methylene dinaphthalene sulfonate and the sodium lignin sulfonate.
7. The method for preparing ultrafine pear stone cell powder according to any one of claims 1 or 3, wherein: in the step (2), the defoaming agent is organosilicon defoaming agent S2100 or tributyl phosphate or a mixture of the two.
8. The method of claim 1, wherein the ultrafine pear stone cell powder is prepared by: in the step (2), the ball milling and crushing time of the planetary ball mill is 60-240 minutes, the ball milling and crushing temperature is 20-70 ℃, and the rotating speed is 200-600 revolutions per minute.
9. The method of claim 1, wherein the ultrafine pear stone cell powder is prepared by: in the step (3), when the suspension is centrifuged, the rotating speed of a centrifuge is 4000-6000 rpm, the washing is water washing, ethanol washing and water washing in sequence, and the temperature of freeze drying is-15 to-30oC. The time is 8-14 h.
CN202010597327.7A 2020-06-28 2020-06-28 Method for preparing superfine pear stone cell powder Pending CN111822106A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1359986A (en) * 2001-12-29 2002-07-24 中国地质大学（武汉） Process for preparing flaky heavy calcium carbonate
CN101121606A (en) * 2007-07-05 2008-02-13 浙江理工大学 Surface modification method for ruthenium in situ wrapping ultramicro high purity Si3N4 powder
CN101215428A (en) * 2008-01-07 2008-07-09 徐州开达精细化工有限公司 Method for preparing ultra-fine reduction dyestuff
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CN104892003A (en) * 2015-05-04 2015-09-09 齐鲁工业大学 Preparation method of alumina-coated hexagonal boron nitride composite powder for self-lubricating cutter material
CN105712339A (en) * 2014-12-01 2016-06-29 江阴碳谷科技有限公司 Physical stripping production method of graphene
CN107057090A (en) * 2017-04-27 2017-08-18 万华化学集团股份有限公司 A kind of preparation method of nylon powder
CN109748510A (en) * 2017-11-02 2019-05-14 吴春燕 A kind of preparation method of hollow glass micropearl
CN111205828A (en) * 2020-01-13 2020-05-29 青岛大学 Ultra-soft gel particle containing ultra-low temperature phase change material and preparation method thereof

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CN101121606A (en) * 2007-07-05 2008-02-13 浙江理工大学 Surface modification method for ruthenium in situ wrapping ultramicro high purity Si3N4 powder
CN101215428A (en) * 2008-01-07 2008-07-09 徐州开达精细化工有限公司 Method for preparing ultra-fine reduction dyestuff
CN104095798A (en) * 2014-06-19 2014-10-15 杭州电子科技大学 Toothpaste containing biological mineralized abradant
CN105712339A (en) * 2014-12-01 2016-06-29 江阴碳谷科技有限公司 Physical stripping production method of graphene
CN104892003A (en) * 2015-05-04 2015-09-09 齐鲁工业大学 Preparation method of alumina-coated hexagonal boron nitride composite powder for self-lubricating cutter material
CN107057090A (en) * 2017-04-27 2017-08-18 万华化学集团股份有限公司 A kind of preparation method of nylon powder
CN109748510A (en) * 2017-11-02 2019-05-14 吴春燕 A kind of preparation method of hollow glass micropearl
CN111205828A (en) * 2020-01-13 2020-05-29 青岛大学 Ultra-soft gel particle containing ultra-low temperature phase change material and preparation method thereof

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