CN1220271A - Method for producing microcrystalline cellulose by sulfating waste cotton velvet - Google Patents
Method for producing microcrystalline cellulose by sulfating waste cotton velvet Download PDFInfo
- Publication number
- CN1220271A CN1220271A CN 98120373 CN98120373A CN1220271A CN 1220271 A CN1220271 A CN 1220271A CN 98120373 CN98120373 CN 98120373 CN 98120373 A CN98120373 A CN 98120373A CN 1220271 A CN1220271 A CN 1220271A
- Authority
- CN
- China
- Prior art keywords
- ageing
- microcrystalline cellulose
- weight
- suede
- acid
- 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
Landscapes
- Processing Of Solid Wastes (AREA)
- Detergent Compositions (AREA)
Abstract
The production method of avicel by using sulfated waste cotton velvet includes the folowing steps: ageing, washing with water, removing impurities, bleaching, declorination treatment, dehydration, oven-drying,pulverizing, screening, checking and packing, and possesses the characteristics of less investment, low cost, reducing dose of chemical reagent and reducing environmental pollution. Said invention is suitable for large-scale industrial production as well as small-batch production.
Description
The present invention relates to make the production method of Microcrystalline Cellulose with sulfated waste cotton velvet.
Microcrystalline Cellulose is a kind of product of white powder, be anisotropic spindle shape aggregate in microscopically observation, it is particle pencil thing, its principal character has three: one, the mean polymerisation degree polymerization degree value that reaches capacity, its mean polymerisation degree DP is between 15-375, and the DP of cotton fibre is about 14000, and the DP of wood-cellulose is about 7000; Its two, have cellulosic patterned features, degree of crystallinity is higher than the protofibril material, the crystalline indice of general cotton pulp Microcrystalline Cellulose is about 0.80, improves 10% approximately than the crystalline indice of raw cotton fiber; Its three, have extremely strong hygroscopicity value, under the high shear with high-speed stirring or homogenizer in water medium, it can be separated into the crystallite that length and width are 0.4 * 0.04 μ m, and can form gelinite rapidly.
The characteristics determined of Microcrystalline Cellulose its in industries such as medicine, food, makeup, process hides and light industry, be with a wide range of applications.As the compressing tablet vehicle that is used for pharmaceutical industry have than traditional starch vehicle take that disintegration power in back is good, drug effect is fast, scattered, and because binding property is good, can direct compression, simplified technical process, improve production efficiency, also can be used for making the medicine of paste or suspension.As in foodstuffs industry, because of it is a natural material, nontoxic, tasteless, as not influence original food look, shape, flavor characteristics, Microcrystalline Cellulose can be used as emulsion and foaming stabiliser, high-temperature stabiliser, non-nutritive weighting material, tackifier, dispersion agent, conformal agent, gelifying agent and ice crystal prevent agent etc.As at used for cosmetic in producing paste or emulsus makeup.In Production of Ceramics, dosing Microcrystalline Cellulose in potter's clay can increase wet base intensity, improve the work in-process rate, and the characteristic merrily and lightheartedly exquisitely carved owing to the burn off cellulosic has, that quality is transparent of the porcelain behind the roast.In synthetic leather is produced, can be used as tackifier and micropore agent.Can be used as weighting agent, catalyst carrier, chemical industry flocculating aids, welding electrode ignition dope and the number of chemical reagent of carbon element transfer paper, carpet cleaner and mould washing composition, plastics and rubber in addition.
The manufacture method of Microcrystalline Cellulose commonly used be with natural cellulose with dilute acid hydrolysis to the limit polymerization degree, again through neutralization, bleaching, washing, dry, pulverize, sieve; Or with natural cellulose with the direct crushing screening of special Highefficientpulverizer; Or use earlier dilute acid hydrolysis, and pulverize, sieve with Highefficientpulverizer again, no matter which kind of method of employing is a raw material with the natural cellulose all, production cost is higher.
China is one and produces cotton big country, produces a large amount of sulfation velveteens in the cotton seed course of processing, be taken as waste for a long time and transport to open-air burning disposal, and not only labor intensive, material resources, and burning produces a large amount of toxic gas pollutant atmospheres.Have the people that it is sprinkled into the saltings in recent years, attempt to improve alkaline soil, but the salt that acid-base neutralisation produces can produce adverse influence to crop growth again, therefore, how developing sulfated waste cotton velvet has become problem anxious to be solved.
China Patent No. ZL92105523.4, name is called " using technology for producing microcrystalline cellulose with sulfated waste cotton velvet " and discloses a kind of with neutralization, the degraded bleaching, oven dry, pulverize, the processing method of sieving, but according to the existing production technology of domestic and international Microcrystalline Cellulose and the inventor is the research and the practice of development of raw materials Microcrystalline Cellulose product for a long time with the sulfated waste cotton velvet, find that this technology can realize in theory, but it is very difficult to be applied to operate in the actual industrial production process, particularly N-process wherein not only consumes a large amount of alkali and heat energy, and it is very high that material is heated to 80 ℃ of facility investments, also strengthened simultaneously production cost, " degraded bleaching " technology wherein is not too reasonable, because in actual production, degrading with SYNTHETIC OPTICAL WHITNER is difficult to control, and seriously influences the stability of quality product.
The inventor has carried out years of researches and has repeatedly practised at the defective that prior art exists, and creates technical scheme of the present invention.
The object of the present invention is to provide a kind of production method, overcome the drawback of prior art, reach the purpose that reduces production costs, improves the quality of products and reduce environmental pollution with sulfated waste cotton velvet manufacturing Microcrystalline Cellulose.
The object of the present invention is achieved like this:
A kind of production method of making Microcrystalline Cellulose with sulfated waste cotton velvet, this method comprises following processing step successively: (one), ageing: sulfated waste cotton velvet is stored in the storehouse, avoid the sunlight direct irradiation, the ageing of degrading is slowly under field conditions (factors) handled, time is 30～700 days, makes ageing acid suede;
(2), washing: divide 2～4 times with the clear water washing to ageing acid suede, remove residual acid, each water consumption is 10～25 times of ageing acid suede weight;
(3), removal of impurities: the ageing acid suede after will washing is removed mechanical impuritys such as sand, cotton seed hull;
(4), bleaching: then bleach processing with the SYNTHETIC OPTICAL WHITNER of concentration 1～15% (weight) under normal temperature condition, the SYNTHETIC OPTICAL WHITNER consumption is 0.5～2 times of the sour suede weight of ageing, and the time is 1～3 hour, to Microcrystalline Cellulose whiteness 〉=60 o'clock only; Wash 1～3 time to PH5～7 with clear water, each water consumption is 10～25 times of ageing acid suede weight;
(5), dechlorination: the dechlorinating agent with 0.1～2.5% (weight) carries out the dechlorination processing to the Microcrystalline Cellulose after bleaching, to remove wherein remaining atomic chlorine, with clear water washing 1～3 time, each water consumption is 10～25 times of ageing acid suede weight, till starch-kalium iodide indicator check nondiscoloration;
(6), dewatered drying: put into the drying unit inner drying after the Microcrystalline Cellulose centrifuge dehydration with described (five), temperature is controlled at 20～150 ℃, ends to moisture＜5% o'clock;
(7), crushing screening: will dry material and pulverize, and sieve with 40～900 purpose screen clothes with pulverizer;
(8), test package: test package according to a conventional method.
Should the used SYNTHETIC OPTICAL WHITNER of (four) bleaching comprise clorox or calcium hypochlorite solution.
Can also then increase after described (five) dechlorination processing from handling, the diaminostilbene sodium sulfonate of use 0.06～0.2% (weight) or product orchid or ultramarine were soaked 1～3 hour.
Be somebody's turn to do the dechlorinating agent that uses in (five) dechlorination processing and comprise sodium thiosulfate (Na
2S
2O
3) or urea.
Major advantage of the present invention is:
1, the used main raw material of the present invention itself is exactly a linters with acid hydrolysis to a certain degree product, production method of the present invention makes full use of wherein remaining acid at ambient temperature after ageing, only need bleaching, washing, dry, pulverizing, sieving to make Microcrystalline Cellulose, not only simplified production process, saved raw material, reduce facility investment, greatly reduced production cost.
2, the present invention has increased the dechlorination processing and has brightened processing, prevents Microcrystalline Cellulose product brightness reversion, has improved the quality of product, and the demand of the higher whiteness that can meet the demands.
The present invention is further described below in conjunction with preferred embodiment and technological process of production figure.
Fig. 1 is technological process of production figure of the present invention.
Consult Fig. 1, it is that sulfated waste cotton velvet is stored in the storehouse that ageing is handled, and avoids sunlight directly according to solarization, utilizes sulfuric acid remaining in the sulfated waste cotton velvet that velveteen is degraded slowly under natural climate.
We know, its granularity of Microcrystalline Cellulose of different purposes is different and has certain distribution, for example, is 60 μ m at the common J422 type of welding rod industry welding rod with the fiber mean particle size of Microcrystalline Cellulose, and size-grade distribution is represented with 32 μ m, 100 μ m and three kinds of sieves of 200 μ m shared percentage ratio of back screenings that sieves:
6010 type high-cellulose welding rods are 130 μ m with the fiber mean particle size, and size-grade distribution is represented as follows with the shared percentage ratio of screenings:
In food industry applications, the edible Microcrystalline Cellulose mean particle size of modification requires less than 10 μ m, and wherein the particle of 1 μ m should account for more than 10% (weight).In synthetic leather was produced, the wet production Synthetic Leather was 30 μ m with the Microcrystalline Cellulose mean particle size, and wherein the granularity of 5 μ m accounts for more than 10% (weight).
From above example as can be seen, the granularity of Microcrystalline Cellulose and distribution thereof are important indicators that characterizes the Microcrystalline Cellulose morphological structure, and the Microcrystalline Cellulose with different shape structure then has different purposes.
Therefore, explore different seasons, different temperature and different factors such as the time Changing Pattern to fiber ageing hydrolysis influence, the Microcrystalline Cellulose product of producing forecast quality is a key problem in technology of the present invention.The ageing treatment time, and different, digestion time was shorter when summer temperature is higher with different seasons, different temperature variation, and digestion time was longer when temperature was low in the winter time.Digestion time is 30～700 days during actual production, requires the Warehouse Keeper to carry out detailed record to batch, the place of production, the entry time of every batch of raw material.
Cotton seed process period, the collection of sulfated waste cotton velvet was also concentrated during this period of time generally in year March in October to the second in every year.For convenience of explanation, we select the raw material of November warehouse-in further to set forth, and for example, in the May of control digestion time to the second year when producing J422 type welding rod with Microcrystalline Cellulose, amount to and can reach granularity requirements in about 180 days; And produce 6010 type high-cellulose welding rods with Microcrystalline Cellulose time control digestion time to the second year February, and amount to about 90 days, can reach granularity requirements; As be used for production use for synthetic leather Microcrystalline Cellulose, in the July of control digestion time to the second year, can reach granularity requirements.
Under field conditions (factors), the method of handling with ageing realizes to cellulosic degraded it being maximum invention of the present invention: make full use of sulfuric acid remaining in the waste cotton velvet, do not add any auxiliary agent, reduced raw materials cost, simplified technological process, reduce investment of production equipment, improved the quality of Microcrystalline Cellulose product.
Washing is the residual acid of removing in the sour suede of ageing, can wash 3 times, and PH is reached about 4, and each water consumption is 15 times of ageing acid suede weight, and its concrete grammar is to soak ageing acid suede with clear water, and supernatant liquor is removed in stirring, precipitation hypsokinesis.Removal of impurities is to remove sand, cotton seed hull or other mechanical impurity with centrifugal screen and/or swirler.Bleaching is to use the conventional bleaching method, uses 10% chlorine bleach liquor, and consumption is 1.2 times of ageing acid suede weight, and the time is to end to Microcrystalline Cellulose whiteness 〉=60 in 1.5 hours, with clear water washing 2 times, to PH be 5.Sodium thiosulfate (the Na that adds 1.5% (weight) is handled in dechlorination
2S
2O
3) or urea, normal temperature stirs down, time is 1 hour, purpose is in order to remove remaining chlorine, prevent the Microcrystalline Cellulose brightness reversion, brighten the diaminostilbene sodium sulfonate dipping of handling 0.03% (weight) commonly used, purpose is for the whiteness that improves product (usefulness during just whiteness had relatively high expectations, when less demanding can).Dewatered drying is with after the centrifuge dehydration, will dry material and evenly put into drying unit, 40 ℃, about 10 hours time, to water content＜5% only.Crushing screening is to utilize Universalpulverizer will dry material to carry out pulverization process, then according to the service requirements difference, select the screen cloth of different apertures to sieve, screen sizes is selected generally between 40～900 orders, can be with 80 purpose screen clothes as the Microcrystalline Cellulose of welding electrode special use; The agent of synthetic leather micropore can be with 400 purpose screen clothes with Microcrystalline Cellulose.Product is packed warehouse-in with test qualified back of ordinary method.
Production method of the present invention has been improved the operation of using residual acid in the alkali neutralisation of sulphuric acid waste cotton velvet in the prior art, adopt the ageing treatment process of slowly degrading under the natural condition, reduce raw materials cost and heat energy loss, simplified production technique, improved the stability of production and the quality of product; The present invention has increased the dechlorination processing and has brightened processing, prevents the product brightness reversion, guarantees that product has higher whiteness, has further improved quality product.
Production method of the present invention makes the waste water of discharging meet discharge standard, no owing to greatly reduced the industrial chemicals use amount Can cause environmental pollution; Production equipment of the present invention is simple, is fit to large-scale industrial production, also suitable do things simply and thriftily small quantities of Amount is produced, and has that small investment, cost are low, the characteristics of instant effect, for the industries such as light industry, chemical industry provide colory little The plain product of crystal fiber.
Claims (4)
1, a kind of production method with sulfated waste cotton velvet manufacturing Microcrystalline Cellulose is characterized in that this method comprises following processing step successively:
(1), ageing: sulfated waste cotton velvet is stored in the storehouse, avoids the sunlight direct irradiation, the ageing of degrading is slowly under field conditions (factors) handled, and the time is 30～700 days, makes ageing acid suede;
(2), washing: divide 2～4 times with the clear water washing to ageing acid suede, remove residual acid, each water consumption is 10～25 times of ageing acid suede weight;
(3), removal of impurities: the ageing acid suede after will washing is removed mechanical impuritys such as sand, cotton seed hull;
(4), bleaching: then bleach processing with the SYNTHETIC OPTICAL WHITNER of concentration 1～15% (weight) under normal temperature condition, the SYNTHETIC OPTICAL WHITNER consumption is 0.5～2 times of the sour suede weight of ageing, and the time is 1～3 hour, to Microcrystalline Cellulose whiteness 〉=60 o'clock only; Wash 1～3 time to PH5～7 with clear water, each water consumption is 10～25 times of ageing acid suede weight;
(5), dechlorination: the dechlorinating agent with 0.1～2.5% (weight) carries out the dechlorination processing to the Microcrystalline Cellulose after bleaching, to remove wherein remaining atomic chlorine, with clear water washing 1～3 time, each water consumption is 10～25 times of ageing acid suede weight, till starch-kalium iodide indicator check nondiscoloration;
(6), dewatered drying: put into the drying unit inner drying after the Microcrystalline Cellulose centrifuge dehydration with described (five), temperature is controlled at 20～150 ℃, ends to moisture＜5% o'clock;
(7), crushing screening: will dry material and pulverize, and sieve with 40～900 purpose screen clothes with pulverizer;
(8), test package: test package according to a conventional method.
2, production method according to claim 1 is characterized in that the used SYNTHETIC OPTICAL WHITNER of these (four) bleaching comprises clorox or calcium hypochlorite solution.
3, production method according to claim 1 is characterized in that can also then brightening processing after described (five) dechlorination processing, and the diaminostilbene sodium sulfonate of use 0.06～0.2% (weight) or product orchid or ultramarine were soaked 1～3 hour.
4, production method according to claim 1 is characterized in that the dechlorinating agent that uses in this (five) dechlorination processing comprises sodium thiosulfate (Na
2S
2O
3) or urea.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98120373A CN1075514C (en) | 1997-10-13 | 1998-10-09 | Method for producing microcrystalline cellulose by sulfating waste cotton velvet |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97119006.2 | 1997-10-13 | ||
| CN97119006 | 1997-10-13 | ||
| CN98120373A CN1075514C (en) | 1997-10-13 | 1998-10-09 | Method for producing microcrystalline cellulose by sulfating waste cotton velvet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1220271A true CN1220271A (en) | 1999-06-23 |
| CN1075514C CN1075514C (en) | 2001-11-28 |
Family
ID=25744377
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98120373A Expired - Fee Related CN1075514C (en) | 1997-10-13 | 1998-10-09 | Method for producing microcrystalline cellulose by sulfating waste cotton velvet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1075514C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295250C (en) * | 2004-11-18 | 2007-01-17 | 上海大学 | Preparation method of sweet potato diet microcrystal cellulose |
| US20120223165A1 (en) * | 2011-03-02 | 2012-09-06 | Liliana Graciela Buente Alonso | Method for Obtaining Microcrystalline Cellulose from Residues Derived from Acid Delinting of Cottonseed |
| CN103122592A (en) * | 2011-11-18 | 2013-05-29 | 奎屯新大陆化学有限公司 | Method for preparing microcrystalline cellulose from waste cotton |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101067287B (en) * | 2007-05-31 | 2011-07-27 | 王光建 | Producing technology for microcrystalline cellulose with waste acid cotton linter |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS538334B2 (en) * | 1974-01-29 | 1978-03-28 | ||
| JPH06212587A (en) * | 1991-03-11 | 1994-08-02 | New Oji Paper Co Ltd | Production of fine fibrous cellulose |
| CN1037846C (en) * | 1992-07-04 | 1998-03-25 | 苏志刚 | Technology for producing microcrystalline cellulose with sulfated waste cotton velvet |
| JPH07102074A (en) * | 1993-09-30 | 1995-04-18 | Asahi Chem Ind Co Ltd | Method for converting cellulose material into minute particle |
| JP3262917B2 (en) * | 1993-09-30 | 2002-03-04 | 旭化成株式会社 | Fine cellulose and its manufacturing method |
| JP3036354B2 (en) * | 1994-05-17 | 2000-04-24 | 特種製紙株式会社 | Method for producing fine fibrillated cellulose |
| JP4850996B2 (en) * | 2000-04-28 | 2012-01-11 | パナソニック株式会社 | Electrode plate unit and battery |
-
1998
- 1998-10-09 CN CN98120373A patent/CN1075514C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295250C (en) * | 2004-11-18 | 2007-01-17 | 上海大学 | Preparation method of sweet potato diet microcrystal cellulose |
| US20120223165A1 (en) * | 2011-03-02 | 2012-09-06 | Liliana Graciela Buente Alonso | Method for Obtaining Microcrystalline Cellulose from Residues Derived from Acid Delinting of Cottonseed |
| CN103122592A (en) * | 2011-11-18 | 2013-05-29 | 奎屯新大陆化学有限公司 | Method for preparing microcrystalline cellulose from waste cotton |
| CN103122592B (en) * | 2011-11-18 | 2015-01-07 | 奎屯新大陆化学有限公司 | Method for preparing microcrystalline cellulose from waste cotton |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1075514C (en) | 2001-11-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104179055B (en) | Grass fiber bio-separation compound formulation | |
| CN102345244A (en) | Pulping and papermaking process through multiple-composition biological enzyme method | |
| CN1049111A (en) | The acid soak acid heat activation of Concave-convex clay rod | |
| CN106917309B (en) | A kind of preparation method of corn stalk stalks of rice, wheat, etc. cellulose short-term training film | |
| CN109629282A (en) | A method of matched using corn stalk raw material preparation true qualities wrapping paper plate and plagiarizes slurry | |
| CN106223087A (en) | A kind of dry method pulping process and equipment | |
| CN107602709A (en) | A kind of carboxymethyl nano cellulose material cleans preparation method | |
| CN107740305A (en) | A kind of method that stalk prepares high-strength corrugated base paper | |
| CN103342826A (en) | Preparation method of chitin nano-fiber/montmorillonite composite membrane material | |
| CN1075514C (en) | Method for producing microcrystalline cellulose by sulfating waste cotton velvet | |
| CN1715556A (en) | Method for pulping and paper-making | |
| CN109868667B (en) | Preparation method of lignin-containing nanocellulose filaments | |
| CN206189186U (en) | Dry process pulping equipment | |
| CN103821030A (en) | Presoak for papermaking and preparation method thereof, and paper industrial packaging production process | |
| CN113502675A (en) | Preparation method and product of mild and green lignin-containing nanocellulose filaments | |
| CN108751191A (en) | The preparation method of activated carbon is produced with bamboo particle | |
| CN106245393B (en) | Vegetation pulp production device | |
| CN105064110A (en) | Cotton linter pulping device and pulping method thereof | |
| CN100359093C (en) | Technology of making paper and paper products by banana fibre | |
| CN1340651A (en) | Process for preparing arc microcrystal cellulose | |
| CN105803841A (en) | Method for improving viscose bamboo pulp reaction performance | |
| CA1124962A (en) | Process of bleaching peat moss and resulting product | |
| CN115418875A (en) | Method for extracting nano-cellulose from water hyacinth | |
| CN1865582A (en) | Cold-immersion mechanical pulping process for xyloid raw materials | |
| CN1037846C (en) | Technology for producing microcrystalline cellulose with sulfated waste cotton velvet |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20011128 Termination date: 20131009 |