CN114988955A - Preparation method of oil for chemical fertilizer anti-caking agent and chemical fertilizer anti-caking agent - Google Patents
Preparation method of oil for chemical fertilizer anti-caking agent and chemical fertilizer anti-caking agent Download PDFInfo
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- CN114988955A CN114988955A CN202210799032.7A CN202210799032A CN114988955A CN 114988955 A CN114988955 A CN 114988955A CN 202210799032 A CN202210799032 A CN 202210799032A CN 114988955 A CN114988955 A CN 114988955A
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- 239000003337 fertilizer Substances 0.000 title claims abstract description 68
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000126 substance Substances 0.000 title claims description 23
- 239000000463 material Substances 0.000 claims abstract description 33
- 238000005886 esterification reaction Methods 0.000 claims abstract description 26
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 18
- 239000000194 fatty acid Substances 0.000 claims abstract description 18
- 229930195729 fatty acid Natural products 0.000 claims abstract description 18
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 17
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 16
- 239000011541 reaction mixture Substances 0.000 claims abstract description 16
- 239000002250 absorbent Substances 0.000 claims abstract description 10
- 230000002745 absorbent Effects 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 4
- -1 di-tert-butyl propane peroxide Chemical class 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- RZEWIYUUNKCGKA-UHFFFAOYSA-N 2-(2-hydroxyethylamino)ethanol;octadecanoic acid Chemical compound OCCNCCO.CCCCCCCCCCCCCCCCCC(O)=O RZEWIYUUNKCGKA-UHFFFAOYSA-N 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 2
- 239000003729 cation exchange resin Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims 1
- 238000011282 treatment Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 25
- 238000012360 testing method Methods 0.000 description 8
- 238000004042 decolorization Methods 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000002981 blocking agent Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical group N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000001692 EU approved anti-caking agent Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 229960001866 silicon dioxide Drugs 0.000 description 2
- 239000003930 superacid Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000001412 amines Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003712 decolorant Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 125000002485 formyl group Chemical group [H]C(*)=O 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/30—Anti-agglomerating additives; Anti-solidifying additives
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a preparation method of oil for a fertilizer anti-caking agent and the fertilizer anti-caking agent, wherein the preparation method comprises the following steps: (1) taking 30-80 parts by weight of a bottom material produced by fatty acid, 10-30 parts by weight of a bottom material produced by fatty alcohol, 0.2-3.0 parts by weight of a catalyst and 0-10 parts by weight of a water absorbent, and mixing and then carrying out esterification reaction to obtain an esterification reaction mixture; (2) and cooling the esterification reaction mixture, adding 1-20 parts by weight of a decolorizing agent, and carrying out decolorizing reaction to obtain the oil for the fertilizer anti-caking agent. The invention does not need to carry out any treatment such as filtration or impurity removal on the bottom materials and the final reaction mixture, and the discharged materials are the oil for the fertilizer anti-caking agent after the treatment of the invention, thereby having very good fertilizer anti-caking effect, simple operation process and good practicability.
Description
Technical Field
The invention relates to the technical field of fertilizers, in particular to a preparation method of oil for a fertilizer anti-caking agent and the fertilizer anti-caking agent.
Background
The fertilizer is an important fertilizer in agricultural production, and can promote the yield increase of crops and the like. And caking is easily generated in the fertilizer storage process, the fertilizer application process of the fertilizer is affected, and the fertilizer application of agricultural machinery cannot be carried out. At present, in order to prevent the fertilizer from caking at home and abroad, an anti-caking agent is coated on the surface of the fertilizer in the fertilizer production process generally so as to solve the problem of caking of the fertilizer.
The fertilizer anticaking agent is mainly prepared from fatty acid ester or fatty alcohol, fatty acid and the like. At present, the price of the raw materials is sharply increased, so that the cost of the anti-caking agent is greatly increased. In order to seek a low-cost substitute, the anti-caking agent is prepared by selecting bottom materials produced by fatty acid and fatty alcohol, the bottom materials of the fatty acid and the fatty alcohol are waste materials of oil chemical plants, but the bottom materials can not play a role in preventing caking of chemical fertilizers when being directly used, and have the problems of high viscosity and deep color, thereby influencing the application in the anti-caking agent for fertilizers.
Disclosure of Invention
The invention mainly aims to provide a preparation method of oil for a fertilizer anti-caking agent and the fertilizer anti-caking agent, and aims to solve the technical problem that a base material produced by fatty acid and fatty alcohol cannot be directly used in the fertilizer anti-caking agent in the prior art.
In order to realize the purpose, the invention provides a preparation method of oil for a fertilizer anti-caking agent, which comprises the following steps:
(1) taking 30-80 parts by weight of a bottom material produced by fatty acid, 10-30 parts by weight of a bottom material produced by fatty alcohol, 0.2-3.0 parts by weight of a catalyst and 0-10 parts by weight of a water absorbent, and mixing and then carrying out esterification reaction to obtain an esterification reaction mixture;
(2) and cooling the esterification reaction mixture, adding 1-20 parts by weight of a decolorizing agent, and carrying out decolorizing reaction to obtain the oil for the fertilizer anti-caking agent.
Further, the catalyst is sulfuric acid, phosphoric acid, organic sulfonic acid and salt thereof, and solid super acid SO 2 4 - /TiO 2 -SiO 2 Any one or a mixture of more than two of sodium methoxide, sodium ethoxide, cation exchange resin and sulfamic acid.
Further, the water absorbent is any one or a mixture of more than two of allochroic silicagel and high water absorption resin.
Further, the decolorizing agent is hydrogen peroxide and derivatives thereof or potassium permanganate, and the hydrogen peroxide and the derivatives thereof are any one or a mixture of more than two of tert-butyl hydroperoxide, dibenzoyl peroxide and di-tert-butyl propane peroxide.
Further, the temperature of the esterification reaction is 60-95 ℃, and the reaction time is 1-3 hours.
Further, the cooling temperature is 45-80 ℃, and the decoloring reaction time is 0.2-5 hours.
The invention also provides a fertilizer anti-caking agent, which comprises the following raw materials in parts by weight: 30-50 parts of oil for the fertilizer anti-caking agent prepared by the preparation method, 5-10 parts of white oil, 10-20 parts of glycerol and 10-25 parts of stearic acid diethanolamine condensate.
The invention has the beneficial effects that:
the invention makes acid substances in the bottom materials produced by fatty acid, mainly alcohol substances in the bottom materials produced by fatty acid and fatty alcohol, mainly fatty alcohol generate esterification reaction to generate ester substances, the catalyst has the function of improving reaction efficiency, the water absorbent is added to absorb water generated by the reaction, the esterification reaction is carried out towards the direction of generating the ester substances, after the esterification reaction is finished, a decolorant is used for oxidation, deep color groups and color-assisting groups such as heterocycle, aldehyde, amine, nitrogen and the like are oxidized into colorless groups, the bottom materials before being processed contain colloid, the viscosity of the bottom materials is very high, the bottom materials are not suitable for being directly used as anti-caking agents of chemical fertilizers, after being processed by the invention, the viscosity is greatly reduced, the problems of color depth and heavy smell are effectively improved, the anti-caking agents of chemical fertilizers can be used, the invention does not need to carry out any filtration or impurity removal and other treatments on the bottom materials and the final reaction mixture, the discharged material is the oil for the fertilizer anti-caking agent after the treatment of the invention, and the invention has good fertilizer anti-caking effect, simple operation process and good practicability.
Detailed Description
The invention is further described below with reference to the following examples:
the various starting materials used in the following examples are all commercially available products known in the art unless otherwise specified. Wherein, the footing material for producing fatty acid is purchased from Shandongxin river new material Co., Ltd, and the footing material for producing fatty alcohol is purchased from Jinan Wei Zheng chemical Co., Ltd. The kinematic viscosity of the heel material produced from fatty acid is 190mm 2 (s) kinematic viscosity of the heel material from fatty alcohol production of 60mm 2 The main components are shown in the following table 1 and table 2:
table 1 base stock major ingredients for fatty acid production
Composition (A) | Content% |
Fatty acids | 75.32 |
Esters as pesticides | 17.90 |
Alkane(s) | 5.83 |
Olefins | 0.95 |
Table 2 base stock major ingredients for fatty alcohol production
Composition (I) | Content% |
Alcohol(s) | 30.85 |
Nitrogen-containing compounds | 8.07 |
Esters as pesticides | 31.54 |
Others | 29.54 |
Example 1
The preparation method of the oil for the fertilizer anti-caking agent comprises the following steps:
(1) mixing 30 parts by weight of a base material produced by fatty acid, 10 parts by weight of a base material produced by fatty alcohol, 0.2 part by weight of phosphoric acid and 1 part by weight of super absorbent resin, and then carrying out esterification reaction at 60 ℃ for 3 hours to obtain an esterification reaction mixture;
(2) and cooling the esterification reaction mixture to 45 ℃, adding dibenzoyl peroxide 1 in parts by weight, and carrying out decolorization reaction for 0.2 hour to obtain the oil for the chemical fertilizer anti-caking agent.
Example 2
The preparation method of the oil for the fertilizer anti-caking agent comprises the following steps:
(1) mixing 55 parts by weight of a base material produced by fatty acid, 20 parts by weight of a base material produced by fatty alcohol, 1.6 parts by weight of sulfuric acid and 5 parts by weight of super absorbent resin, and then carrying out esterification reaction at the temperature of 80 ℃ for 2 hours to obtain an esterification reaction mixture;
(2) and cooling the esterification reaction mixture to 70 ℃, adding 10 parts by weight of tert-butyl hydroperoxide, and carrying out decolorization reaction for 2.6 hours to obtain the oil for the fertilizer anti-caking agent.
Example 3
The preparation method of the oil for the fertilizer anti-caking agent comprises the following steps:
(1) mixing 80 parts by weight of a bottom material produced by fatty acid, 30 parts by weight of a bottom material produced by fatty alcohol, 3.0 parts by weight of sulfamic acid and 10 parts by weight of allochroic silica gel, and then carrying out esterification reaction at the temperature of 95 ℃ for 1 hour to obtain an esterification reaction mixture;
(2) and cooling the esterification reaction mixture to 80 ℃, adding di-tert-butyl propane peroxide 20 in parts by weight, and carrying out decolorization reaction for 5 hours to obtain the oil for the fertilizer anti-caking agent.
Example 4
The preparation method of the oil for the fertilizer anti-caking agent comprises the following steps:
(1) taking a bottom material 55 produced by fatty acid, a bottom material 20 produced by fatty alcohol, and solid super acid SO according to parts by weight 2 4 - /TiO 2 -SiO 2 1.6 and the super absorbent resin 5, and carrying out esterification reaction at the temperature of 80 ℃ for 2 hours to obtain an esterification reaction mixture;
(2) and cooling the esterification reaction mixture to 70 ℃, adding potassium permanganate 10 according to the weight part, and carrying out decolorization reaction for 2.6 hours to obtain the oil for the chemical fertilizer anti-caking agent.
Example 5
Performance testing of oil for chemical fertilizer anti-blocking agent
The oil for the fertilizer anti-caking agent prepared in the above example was subjected to component detection and viscosity test, and the results are shown in table 3:
TABLE 3 anti-caking agent for chemical fertilizers oil essential component
The oil for the fertilizer anti-caking agent prepared in the embodiment is prepared into a fertilizer anti-caking agent sample according to the following weight formula: 0-50% of the oil for the fertilizer anti-caking agent prepared in the embodiment 2, and the balance of a mixture of white oil, glycerol and stearic acid diethanolamine in a ratio of 1:2: 2.5.
Then, performing a fertilizer anti-caking test, wherein the test method comprises the following steps: adding a chemical fertilizer into a medical coating machine, heating to 50-60 ℃, adding a chemical fertilizer anti-caking agent sample accounting for 1% of the weight of the chemical fertilizer, coating for 5-10 minutes, discharging, packaging by small plastic self-sealing bags filled with about 100 g of the chemical fertilizer, packaging 100 g of the chemical fertilizer in each bag, flatly paving on a test bed, pressing the test bed with a thick steel plate weighing 10 kg of the chemical fertilizer, pressing the steel plate with a weight of 50 kg of the chemical fertilizer, removing the weight and the steel plate after 7 days, placing each bag of the chemical fertilizer on a 4-mesh test sieve, screening the materials, weighing the weight, dividing the materials on the sieve by 100 to obtain the caking rate, reducing the value by 1 to obtain the caking rate, wherein the larger the caking rate is better.
The anti-caking test results are shown in table 4:
TABLE 4 anti-caking test results
From the above, the oil for the fertilizer anti-caking agent prepared by the invention has a very good effect of preventing the fertilizer from caking, the base stock before treatment contains colloid, so that the viscosity of the base stock is very high, the base stock is not suitable for being directly used as the fertilizer anti-caking agent, and the viscosity is greatly reduced after the treatment of the invention, so that the oil can be used as the fertilizer anti-caking agent.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A preparation method of oil for a fertilizer anti-caking agent is characterized by comprising the following steps:
(1) taking 30-80 parts by weight of a bottom material produced by fatty acid, 10-30 parts by weight of a bottom material produced by fatty alcohol, 0.2-3.0 parts by weight of a catalyst and 0-10 parts by weight of a water absorbent, and mixing and then carrying out esterification reaction to obtain an esterification reaction mixture;
(2) and cooling the esterification reaction mixture, adding 1-20 parts by weight of a decolorizing agent, and carrying out decolorizing reaction to obtain the oil for the fertilizer anti-caking agent.
2. The method for preparing the oil as claimed in claim 1, wherein the catalyst is sulfuric acid, phosphoric acid, organic sulfonic acid and its salt, solid super acidic SO 2 4 - /TiO 2 -SiO 2 Any one or a mixture of more than two of sodium methoxide, sodium ethoxide, cation exchange resin and sulfamic acid.
3. The method for preparing the oil as claimed in claim 1, wherein the water absorbent is one or a mixture of more than two of allochroic silica gel and super absorbent resin.
4. The method for preparing the oil for the fertilizer anti-caking agent as claimed in claim 1, wherein the decolorizing agent is hydrogen peroxide and its derivatives or potassium permanganate, and the hydrogen peroxide and its derivatives are any one or a mixture of more than two of tert-butyl hydroperoxide, dibenzoyl peroxide and di-tert-butyl propane peroxide.
5. The method for preparing the oil as claimed in any one of claims 1 to 4, wherein the esterification reaction temperature is 60-95 ℃ and the reaction time is 1-3 hours.
6. The method for preparing the oil as claimed in any one of claims 1 to 4, wherein the cooling temperature is 45-80 ℃, and the decolorizing reaction time is 0.2-5 hours.
7. A chemical fertilizer anti-caking agent is characterized by comprising the following raw materials in parts by weight: 30-50 parts of oil for the fertilizer anti-caking agent prepared by the preparation method of any one of claims 1-6, 5-10 parts of white oil, 10-20 parts of glycerol and 10-25 parts of stearic acid diethanolamine condensate.
Priority Applications (1)
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CN202210799032.7A CN114988955B (en) | 2022-07-06 | 2022-07-06 | Preparation method of oil for chemical fertilizer anti-caking agent and chemical fertilizer anti-caking agent |
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CN102050679A (en) * | 2011-01-14 | 2011-05-11 | 福建工程学院 | Straw powder-based anti-blocking agent of compound fertilizer |
CN105801244A (en) * | 2016-03-02 | 2016-07-27 | 中国地质大学(北京) | Environment-friendly oil-soluble anti-caking agent for compound fertilizer and preparation method thereof |
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2022
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CN102050679A (en) * | 2011-01-14 | 2011-05-11 | 福建工程学院 | Straw powder-based anti-blocking agent of compound fertilizer |
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CN109400394A (en) * | 2018-12-29 | 2019-03-01 | 成都云图控股股份有限公司 | A kind of compound fertilizer anticaking agent and preparation method thereof and compound fertilizer as made from it |
CN113929535A (en) * | 2021-12-02 | 2022-01-14 | 安徽富瑞雪化工科技股份有限公司 | Environment-friendly anti-blocking agent for compound fertilizer and preparation method thereof |
Non-Patent Citations (1)
Title |
---|
李德海等, 东北林业大学出版社 * |
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