CN111254703A - Preparation method and application of modified natural plant fiber velvet - Google Patents
Preparation method and application of modified natural plant fiber velvet Download PDFInfo
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Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/13—Alginic acid or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/08—Organic compounds
- D06M10/10—Macromolecular compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Paper (AREA)
Abstract
The invention provides a preparation method of modified natural plant fiber velvet for oil absorption, the natural plant fiber velvet prepared by the method has a hydrophobic surface, is not easy to rot, and has good oil absorption, and the preparation method is characterized by comprising the following steps: (a) pulverizing natural plant fiber, grinding, pulping in water solution with pH of above 10, filtering, and drying; (b) filling a high molecular weight and low molecular weight natural high molecular surfactant into a closed container, wherein the ratio of the high molecular weight to the low molecular weight is 1:1, filling CO2 into a container at the temperature of 40-120 ℃ and the pressure of 20-29 MPa without contacting the product obtained in the step (a) with a surfactant; (c) after swelling reaction for a certain time, quickly releasing pressure to obtain the modified natural plant fiber velvet.
Description
Technical Field
The invention relates to a preparation method of natural plant fiber down, in particular to a preparation method and application of modified natural plant fiber down for oil absorption.
Background
In recent years, oil leakage events at sea and on road pipelines frequently occur, oil pollution from food production, catering industry, petrochemical industry, oil exploitation and the like is serious, the oil substances have extremely strong destructiveness on increasingly fragile ecology and environment, for example, crude oil has poor biodegradability in natural environment, and serious water pollution and soil pollution can be caused after long-term retention. How to deal with these contaminations will be a big problem we need to solve at present. Currently, many methods have been used to clean petroleum contaminated areas, such as mechanical extraction, in situ combustion, chemical degradation. The oil absorption material is an efficient, convenient and safe method for treating oil leakage, and is one of the most common methods for treating oil leakage at present. The oil absorption material can not only convert oil pollutants from liquid state to solid state or semi-solid state, which is convenient for the subsequent conventional method treatment, but also absorb oil spill as much as possible, thereby reducing the environmental hazard and simultaneously recovering resources.
Commercially available oil absorbing materials are mainly classified into three major categories, that is, naturally occurring organic oil absorbing materials, organic oil absorbing materials by chemical synthesis, and inorganic mineral materials. The inorganic mineral materials include clay, diatomite, graphite, perlite, silicon dioxide and the like, and have the advantages of low price and safety, but the inorganic mineral materials have low oil absorption, high transportation cost, water absorption, large volume and non-flammability and non-disposability. Currently, the most common practical applications are organic synthetic materials, which have advantages over other types of materials, including: strong oleophylic action, good adsorption performance and higher floating performance. But has the main disadvantages of nonbiodegradability or high biodegradation cost and poor regeneration effect. The organic natural oil absorption material mainly depends on the gaps of the material, absorbs oil through the fiber surface and the capillary principle, and has various varieties, such as wheat straws, corn cobs, wood fibers, peat swamp, kapok, kenaf, bark and the like which are used as oil spill removal adsorbents in oil spill repair, wherein the oil absorption rate of most materials is higher than that of organic synthetic resin, and the natural adsorbents have the advantages of wide sources, economy, practicability, no toxicity, no harm, biodegradability and the like. However, due to the large amount of hydroxyl contained in the cellulose, the materials generally have the defects of poor floatability, water absorption, easy moisture or decay and the like while absorbing oil, so that the application of the materials is limited to a great extent.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of modified natural plant fiber velvet for oil absorption, and the natural plant fiber velvet prepared by the method has a hydrophobic surface, is not easy to rot and simultaneously has good oil absorption.
The invention provides a preparation method of modified natural plant fiber down for oil absorption, which is characterized by comprising the following steps:
(a) pulverizing natural plant fiber, grinding, pulping in water solution with pH of above 10, filtering, and drying;
(b) filling a high molecular weight and low molecular weight natural high molecular surfactant into a closed container, wherein the ratio of the high molecular weight to the low molecular weight is 1:1, filling CO2 into a container at the temperature of 40-120 ℃ and the pressure of 20-29 MPa without contacting the product obtained in the step (a) with a surfactant;
(c) after swelling reaction for a certain time, quickly releasing pressure to obtain the modified natural plant fiber velvet.
The natural plant fiber substrate comprises any one or combination of more than two of wheat straw, rice straw, corn stalk, leaf mold, cattail fiber, peat methane, Lankoubao leaf, lignin, traditional Chinese medicine residue, wood powder, cotton stalk, coconut husk and kenaf; and/or the natural polymer surfactant comprises any one or the combination of more than two of sodium alginate, cellulose nitrate, cellulose acetate butyrate, cellulose xanthate, methyl cellulose, carboxymethyl cellulose, ethyl cellulose, hydroxyethyl cellulose, cyanoethyl cellulose, hydroxypropyl methyl cellulose, gelatin, egg white and cheese protein.
Further, the pulverization grinding includes at least: and grinding and crushing the natural plant fiber base material at room temperature, and respectively screening by using a screening device with 50-150 meshes to obtain natural plant fiber particles.
Further, the beating includes at least: preparing the natural plant fiber particles into plant fiber oven-dried pulp, adding hot water for mixing, adjusting the pH to be more than 10, and pulping under the condition that the pulp concentration is controlled to be 2-10 wt%, wherein the pulping time is 10-120 min, so as to obtain the natural plant fiber pulp.
Further, the natural high molecular surfactant with high molecular weight has the weight average molecular weight of 200000-1000000 Da.
Further, the weight average molecular weight of the low molecular weight high molecular weight surfactant is 15000-50000 Da. The natural plant fiber is physically modified by adding two surfactants with molecular weights, and a hydrophobic natural polymer film is formed on at least the surface of the natural plant fiber substrate, so that the modified natural plant fiber oil absorbent is obtained, wherein the hydrophobic natural polymer film has a multi-level nanometer microstructure. The ratio of high molecular weight to low molecular weight is 1:1, and the optimal hydrophobic polymer film can be obtained under the condition.
Furthermore, the volume of the added macromolecular surfactant accounts for 2.5-5% of the volume of the reaction container.
Further, the supercritical conditions were 80 ℃ and 25.0 MPa. Under this condition, the product can have optimal hydrophobic and other properties.
The invention also provides an application of the modified natural plant fiber down prepared by the method in water body purification or oil stain adsorption. Further, the use comprises: the method comprises the steps of treating floating oil pollution on the surfaces of water bodies in sea, river and lake, purifying industrial sewage enriched with partial oil products, treating organic solvent and domestic kitchen waste oil, adsorbing oil stains on traffic pavements and the like.
The preparation method of the modified natural plant fiber velvet provided by the invention is simple and easy to implement, wide in raw material source, low in cost, green and environment-friendly, natural product fibers and natural products are selected for all fibers, solvents and surfactants, the natural plant fibers are renewable resources, green and environment-friendly, good in biodegradability, free of secondary pollution, free of toxic and harmful organic synthetic compounds, 100% of the natural plant fiber velvet can be buried or regenerated at a later stage, and subjected to directional modification through physical (crushing, grinding, pulping, drying, dipping and the like) means, so that a series of natural plant fiber velvet with excellent oil absorption performance is prepared;
the preparation method of the modified natural plant fiber oil absorbent provided by the invention uses natural surfactants with different molecular weights, can construct a large-medium-small multi-stage and multi-level nanometer microstructure on the fiber surface of natural plant fiber velvet, and concretely, a larger structure in the multi-stage structure is constructed by a high molecular weight natural product, a smaller microstructure in the multi-stage structure is constructed by a low molecular weight natural product, and the multi-stage structure is realized by a supercritical condition, so that the oil absorption is favorably improved in the next step;
according to the method, natural fibers are subjected to roughening and fine fibrillation (devillicate fibrillation) through a pulping technology in a strong alkaline solution, swelling reaction is performed under a supercritical condition, and pressure is rapidly released, so that fine microfibrillation is further realized and is dispersed into fiber fluff, the specific surface area of the surface of an oil absorption material is favorably improved, and the corrosion resistance of the fibers is improved through a supercritical reaction;
compared with the traditional inorganic and organic adsorbents, the modified natural plant fiber velvet has the advantages of high hydrophobicity, strong lipophilicity, high oil absorption rate, high adsorption rate, good oil-water selectivity, easiness in transportation and storage, good floatability, high oil retention rate, greenness, no toxicity, good biodegradability and the like, the oil absorption effect can reach more than ten times of the self weight, oil bodies and the oil absorbents can be separated and repeatedly utilized in a squeezing mode, the operation cost is low, and the modified natural plant fiber velvet is economic and environment-friendly;
the modified natural plant fiber velvet obtained by the invention can be widely applied to the treatment of floating oil pollution on the surfaces of water bodies in sea, river and lake, the purification of industrial sewage with part of oil products enriched, the leakage of toxic organic solvents and the treatment of grease in domestic kitchens, and can also adsorb oil stains on traffic pavements, grounds and the like.
In view of the defects of the prior art, in order to avoid secondary pollution caused in the oil spill treatment process, the preparation method of the natural plant fiber velvet provided by the invention is mainly used for carrying out supercritical modification on natural organic natural plant materials which are good in biocompatibility, easy to biodegrade and low in cost to prepare an efficient and low-cost oil spill treatment material, and the characteristics of high oil absorption rate, low water absorption and the like are achieved by enhancing the hydrophobicity and lipophilicity of fibers and increasing the porosity and specific surface area of the material through dispersing the fibers, so that the standard of practical application requirements is further met.
Detailed Description
Example 1 (1) crushing and grinding: 100g of natural wheat straw fibril was ground and pulverized at room temperature, and sieved with a 50-mesh sieve to obtain 95g of natural wheat straw fibril for use. (2) pulping: adopting vegetable fiber oven-dried pulp made of 95g of natural wheat straw fibril, adding 1000mL of hot water for mixing, adding NaOH to adjust the pH value to 10 to help the fiber to be swelled, and pulping under the condition of controlling the concentration of the pulp to be 8.7 percent for 60min to obtain the natural wheat straw fibril pulp. (3) drying: drying the natural wheat straw fibril pulp at 105 deg.C for 12h to constant weight, taking out and sealing to obtain 80g of natural wheat straw fibril. (4) Adding 5g sodium alginate (with high molecular weight of 500000Da) and 5g sodium alginate (with low molecular weight of 30000Da) into 200mL water, mixing, stirring for 40min to dissolve completely, adding part of the mixture into a sealed reaction kettle, adding natural wheat straw fibril, and introducing CO at 80 deg.C and 25.0MPa without contacting with each other2And after reacting for 1h, quickly relieving pressure to obtain the modified natural plant fiber velvet.
Example 2
The preparation was carried out in the same manner as in example 1, except that the supercritical reaction temperature was 40 ℃.
Example 3
The preparation was carried out in the same manner as in example 1, except that the supercritical reaction temperature was 120 ℃.
Comparative example 1
The preparation was carried out in the same manner as in example 1, except that the supercritical reaction temperature was 150 ℃.
Comparative example 2
The preparation was carried out in the same manner as in example 1, except that the supercritical reaction temperature was 20 ℃.
Comparative example 3
The same preparation as in example 1 was carried out, except that 7.5g of sodium alginate (high molecular weight of 500000Da) and 2.5g of sodium alginate (low molecular weight of 30000Da) were added.
Comparative example 4
The same preparation as in example 1 was carried out, except that 2.5g of sodium alginate (high molecular weight of 500000Da) and 7.5g of sodium alginate (low molecular weight of 30000Da) were added.
Comparative example 5
The same preparation as in example 1 was conducted except that the pH was adjusted to 7 during beating.
Comparative example 6
The same preparation as in example 1 was carried out except that step 4 was not carried out.
Comparative example 7
(1) Crushing and grinding: 100g of natural wheat straw fibril was ground and pulverized at room temperature, and sieved with a 50-mesh sieve to obtain 95g of natural wheat straw fibril for use. (2) pulping: adopting vegetable fiber oven-dried pulp made of 95g of natural wheat straw fibril, adding 1000mL of hot water for mixing, adding NaOH to adjust the pH value to 10 to help the fiber to be swelled, and pulping under the condition of controlling the concentration of the pulp to be 8.7 percent for 60min to obtain the natural wheat straw fibril pulp. (3) drying: drying the natural wheat straw fibril pulp at 105 deg.C for 12h to constant weight, taking out and sealing to obtain 80g of natural wheat straw fibril. And (4) respectively adding 5g of sodium alginate (with the high molecular weight of 500000Da) and 5g of sodium alginate (with the low molecular weight of 30000Da) into 200mL of water, uniformly mixing and stirring for 40min to fully dissolve the sodium alginate and the water, sequentially immersing the natural wheat straw fibril into the solutions with the two molecular weights for 1h, and drying to obtain the product.
The method for detecting the oil absorption performance of the modified natural plant fiber oil absorbent obtained in the embodiment of the invention comprises the following steps: pouring 10mL of oil substance (one or more of petroleum, corn oil, diesel oil, gasoline or toluene) into a beaker containing 80mL of water, layering the oil substance and the oil substance, repeatedly preparing a multi-cup oil-water layering system, pouring the modified oil absorbent obtained in the embodiment of the invention into the beaker, absorbing oil for 5-30 min, and observing and recording the oil absorption effect.
Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | Comparative example 7 | |
Oil absorption (g/g) | 15.6 | 11.3 | 12.7 | 9.3 | 8.9 | 12.1 | 10.5 | 8.0 | 6.2 | 8.1 |
Comparing examples 1,2 and 3 with comparative examples 1 and 2, it can be seen that the supercritical temperature has a large influence on the final performance, presumably because the supercritical temperature will influence the modification amount of the polymer on the fiber surface, and excessively high or low temperature is not favorable for the adsorption of the polymer on the surface. Comparing example 1 with comparative examples 3,4, it was found that the ratio of high molecular weight to low molecular weight is preferably 1: it is presumed that the ratio of the two components makes the multilevel microstructure formed on the surface denser and denser. Comparing example 1 with comparative example 5, it was found that pH 7 during beating resulted in insufficient degree of dispersion and refinement of the fibers, thereby affecting the specific surface area of the product and ultimately the performance. Comparing example 1 and comparative example 6, it was found that the fiber not subjected to polymer modification had a certain oil absorption rate, but it was also found to have strong water absorption during the test. Comparing example 1 and comparative example 7, it was found that the oil absorption rate of the fiber, which was not modified by the supercritical method but by the direct impregnation method, was decreased.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, which are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and therefore, the protection scope of the present invention is not limited thereby. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (8)
1. A preparation method of modified natural plant fiber fluff for oil absorption is characterized by comprising the following steps:
(a) pulverizing natural plant fiber, grinding, pulping in water solution with pH of above 10, filtering, and drying;
(b) filling natural high molecular weight and low molecular weight high molecular weight surfactants into a closed container, wherein the ratio of the high molecular weight to the low molecular weight is 1:1, so that the product obtained in the step (a) is not contacted with the surfactants, and filling CO2 into the container at the temperature of 40-120 ℃ and under the pressure of 20-29 MPa;
(c) after swelling reaction for a certain time, quickly releasing pressure to obtain the modified natural plant fiber velvet.
2. The method of claim 1, wherein the pulverizing and grinding comprises at least: and grinding and crushing the natural plant fiber base material at room temperature, and respectively screening by using a screening device with 50-150 meshes to obtain natural plant fiber particles.
3. The method for preparing modified natural plant fiber fluff according to claim 2, wherein said beating comprises at least: preparing the natural plant fiber particles into plant fiber oven-dried pulp, adding hot water for mixing, adjusting the pH to be more than 10, and pulping under the condition that the pulp concentration is controlled to be 2-10 wt%, wherein the pulping time is 10-120 min, so as to obtain the natural plant fiber pulp.
4. The method of claim 1, wherein the natural polymer surfactant with high molecular weight has a weight average molecular weight of 200000 to 1000000 Da.
5. The method for preparing modified natural plant fiber fluff according to claim 1, wherein the low-molecular-weight polymeric surfactant has a weight-average molecular weight of 15000 to 50000 Da.
6. The method for preparing modified natural plant fiber fluff according to claim 1, wherein the polymeric surfactant is added in an amount of 2.5 to 5% by volume based on the volume of the reaction vessel.
7. The method of claim 1, wherein the supercritical conditions are 80 ℃ and 25.0 MPa.
8. Use in water purification or oil pollution adsorption by using modified natural plant fiber fluff prepared by the method of any one of claims 1 to 7.
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