CN115536632B - Ionic topping agent and application thereof - Google Patents

Ionic topping agent and application thereof Download PDF

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Publication number
CN115536632B
CN115536632B CN202211155380.7A CN202211155380A CN115536632B CN 115536632 B CN115536632 B CN 115536632B CN 202211155380 A CN202211155380 A CN 202211155380A CN 115536632 B CN115536632 B CN 115536632B
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ionic
topping
cotton
comparative example
chlormequat chloride
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CN115536632A (en
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董红强
肖海兵
纪宇曦
文卿琳
刘杰
万素梅
陈国栋
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Tarim University
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Tarim University
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D339/00Heterocyclic compounds containing rings having two sulfur atoms as the only ring hetero atoms
    • C07D339/02Five-membered rings
    • C07D339/04Five-membered rings having the hetero atoms in positions 1 and 2, e.g. lipoic acid
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/24Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with two or more hetero atoms
    • A01N43/26Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with two or more hetero atoms five-membered rings
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01PBIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P21/00Plant growth regulators

Abstract

The invention discloses an ionic topping agent and application thereof, belonging to the technical field of pesticides. The ionic topping agent comprises the following effective components in percentage by weight:the ionic topping agent provided by the invention can improve the high temperature resistance of cotton, reduce the risk of chemical injury, has simple preparation process, simple use and low input cost, greatly reduces the cotton planting cost of cotton farmers, and improves the degree of mechanized operation.

Description

Ionic topping agent and application thereof
Technical Field
The invention belongs to the technical field of pesticides, and particularly relates to an ionic topping agent and application thereof.
Background
The cotton has infinite growth habit, and under a certain temperature condition, the tip continuously grows and stretches, and new stems, leaves and fruit branches are continuously differentiated. If any of them grows, the vegetative growth phase of cotton is prolonged and the maturity is late. Topping is a central link in cotton pruning, and can eliminate the growth advantage of cotton tops, regulate the transportation direction of substances such as water and nutrients in the body, enable more nutrients to be supplied to reproductive organs for growth, reduce the bare consumption of water and fertilizer by invalid fruit branches, promote early fruiting and multi-node ringing of cotton plants, reduce falling off and the like, and have obvious effects of increasing yield and income. The traditional cotton topping is to manually pinch off the growing points of main cotton stems, so that the workload is large and the timeliness is poor. Although the manual topping is good in effect, a large amount of labor force is required, the labor intensity is high, the efficiency is low, and the topping speed is low, so that the yield can be influenced if cotton cannot be topped in time in a proper time. Due to the shortage of labor resources in recent years, the problems of increase of labor cost and the like seriously restrict the realization of the whole mechanization and scale of the cotton industry.
In order to replace the traditional topping mode which is time-consuming and labor-consuming, people try to develop topping machines, a Mala cotton topping machine is developed by agricultural machinery system of the first eighth agricultural college in the 60 th century, and in recent years, a group control type cotton topping machine is developed by Shihe university, but the cotton topping machine cannot be effectively popularized due to the influences of various adverse factors such as large individual difference of cotton, uneven cotton fields, yield reduction and the like. Researchers have also carried out experiments in which chemical agents control the top advantages of cotton, li Xinyu et al (2001) carried out experiments in which long staple cotton chemical capping was used instead of manual capping with single agents, and the results indicate that the replacement of manual capping with chemical capping can reduce the labor intensity, improve the working efficiency and have the potential of improving the yield. However, the single use of the mepiquat chloride has too short duration to well meet the production requirements, and especially the secondary overgrowth phenomenon of upland cotton is easy to occur. The invention relates to a cotton pruning synergist, which is mainly compounded by using the tobacco bud inhibitor flumetralin and mepiquat chloride, and controls the growth of main stems and side branches of cotton through leaf surface spraying, so that the plant is compact, but the persistence is shorter, the later-stage turning of the cotton is easy to cause, and the boll opening is delayed. Zhao Jiang et al (2012) perform basic control on the combination of the mepiquat chloride and the slow release agent (Mepiquat chloride) in the early flowering period, mix the mepiquat chloride and chlormequat chloride for topping in the cotton full flowering period, and spray the mepiquat chloride again for stable plant type control after 3-15 days. The result shows that the method can realize the self-capping of cotton and improve the uniformity of topping of cotton fields, but the pesticide application is complicated, and single yield fluctuates. Chen Xiushuang (2009) the method uses chlormequat chloride to carry out leaf surface spraying to control the growth of the top end of cotton, and results show that the method can realize self capping of cotton, can ensure the capping quality by three times of pesticide application, can effectively control the plant height and the length of branches of cotton, ensure compact plant type of cotton, improve the ventilation and light transmission condition of fields, reduce plant height, shorten branches of fruit, increase the number of flowers before frost, the flower yield before frost and the flower rate before frost, have no obvious influence on the number of bolls, the weight of bolls and the quality of cotton of a single plant, have no phytotoxicity on the safety of cotton, but have extremely high Wen Tianqi at later stage, easily cause the fragility and stiffness of the leaves and the thickening of boll skin, and have great influence on capping peaches. One chlorine atom of chlormequat chloride inhibits stem and leaf elongation, is easy to cause brittleness and rigidity, and cotton boll skin thickens the leaves, and the other chlorine atom promotes reproductive growth, so that the weight of bolls is increased, and the quality is improved. The optimum temperature for cotton boll development is about 30 ℃ and the upper limit temperature is about 35 ℃. In agricultural production, bolls (bolls flowering on days 7, 16 to 8, 15) are the largest among the three bolls, and are the main components of cotton yield. However, the upper limit temperature of July in Xinjiang is about 10d above 35 ℃, under the condition of continuous strong illumination and high temperature forced, the respiration of cotton is aggravated, the cotton is easy to be damaged by oxidization, the pollen activity is reduced, and a large number of bolls are caused to fall off; and the quality of cotton seed cotton single bell, the seed finger and the kernel indication are obviously reduced, the fiber length, the fiber strength and the micronaire value grade are reduced, the yield and the quality of southern Xinjiang cotton are greatly influenced, and the high-temperature oxidation is a main factor influencing the yield and the quality of cotton.
Disclosure of Invention
In order to solve the technical problems, the invention carries out intensive research on the phytotoxicity problems of blade embrittlement and the like caused by chlormequat chloride, and discovers that chlormequat chloride and lipoic acid ionic liquid containing one chloride ion can be generated by the reaction of an anion material (lipoic acid) resisting high-temperature oxidation and chlormequat chloride, and the material has high safety to cotton and can improve the oxidation resistance of cotton under extreme high-temperature stress.
The invention aims to provide an ionic topping agent and application thereof, and the specific technical scheme is as follows:
the first aspect of the invention provides an ionic topping agent, which has the following structural formula:
further, the raw materials for preparing the ionic topping agent comprise chlormequat chloride and lipoic acid.
Further, the ionic topping agent is prepared by acid-base neutralization reaction of chlormequat chloride quaternary ammonium base and lipoic acid; alternatively, the ionic topping agent is prepared by ion exchange reaction of chlormequat chloride and lipoate.
Further, chlormequat chloride and inorganic alkali are placed into an anhydrous organic solvent for reaction, and inorganic salt precipitation is filtered to obtain chlormequat chloride quaternary ammonium alkali solution.
Further, the inorganic base comprises one or more of potassium hydroxide, sodium hydroxide, barium hydroxide, calcium hydroxide, aluminum hydroxide, lithium hydroxide or magnesium hydroxide, preferably potassium hydroxide;
the lipoic acid salt comprises one or more of lipoic acid potassium salt, lipoic acid sodium salt, lipoic acid aluminum salt and lipoic acid magnesium salt.
Further, the molar ratio of lipoic acid to chlormequat chloride is 1 (0.2-2), preferably 1 (0.8-1), more preferably 1:1.
further, the acid-base neutralization reaction or ion exchange reaction is carried out for 1 to 4 hours, preferably 2 to 3 hours.
Further, the temperature of the acid-base neutralization reaction or the ion exchange reaction is 20℃to 80℃and preferably 20℃to 50℃such as 20℃22℃24℃25℃26℃28℃30℃40 ℃.
The second aspect of the invention provides application of the ionic topping agent, wherein the ionic topping agent is a high-temperature oxidation resistant ionic cotton topping agent and is used for improving high-temperature oxidation resistance of cotton.
The beneficial effects of the invention are as follows:
(1) The lipoic acid is selected as the carrier of the ionic pesticide slow release agent, has excellent effect, has strong high-temperature oxidation resistance, is slightly soluble in water, is easily soluble in organic solvents such as ethanol, diethyl ether and the like, can directly play a role in scavenging free radicals such as hydroxyl free radicals, singlet oxygen and the like after entering cells, thereby improving the high-temperature oxidation resistance of plants, and can be prepared into ionic liquid which is easily soluble in water, thereby improving the utilization rate of active ingredients of the medicine. Compared with chlormequat chloride single dosage, the ionic topping agent provided by the invention has better biocompatibility, and has the advantages of improving the utilization rate of pesticide active ingredients, reducing the risk of phytotoxicity and improving the cotton production benefit.
(2) The ionic topping agent provided by the invention can improve the cotton resistanceThe high temperature capability reduces the risk of drug injury, and has simple preparation process, simple use and low input cost (120 hm) -2 ) The cotton planting cost of cotton growers is greatly reduced, the mechanized operation degree is improved, the average unit yield is leveled with the manual topping, and the time, the labor, the money and the labor are saved.
Drawings
FIG. 1 shows the results of chlormequat chloride lipoic acid prepared by the acid-base neutralization reaction of example 1, comparative example 1 (chlormequat chloride single dosage), comparative example 2 (chlormequat chloride salicylate) data comparison of SOD activity, POD activity and MDA content of cotton treated in comparative example 3 (artificial topping) under high temperature stress (weather of day high temperature not less than 35 ℃).
FIG. 2 shows the results of example 2 (chlormequat chloride lipoic acid prepared by ion exchange reaction), comparative example 1 (chlormequat chloride single preparation), comparative example 2 (chlormequat chloride salicylate) data comparison of SOD activity, POD activity and MDA content of cotton treated in comparative example 3 (artificial topping) under high temperature stress (weather of day high temperature not less than 35 ℃).
FIG. 3 shows the results of the acid-base neutralization reaction of chlormequat-lipoic acid prepared in example 3, comparative example 1 (chlormequat-chloride single dosage), comparative example 2 (chlormequat-salicylate) data comparison of SOD activity, POD activity and MDA content of cotton treated in comparative example 3 (artificial topping) under high temperature stress (weather of day high temperature not less than 35 ℃).
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited to the scope of the examples. Unless otherwise indicated, the starting materials employed in the examples of the present invention are those conventionally commercially available in the art.
The invention provides an ionic topping agent, in particular to a high-temperature oxidation resistant ionic cotton topping agent, which comprises the active components of chlormequat lipoic acid ionic liquid. The preparation method comprises the following steps of acid-base neutralization reaction or ion exchange reaction:
acid-base neutralization reaction: quaternary ammonium base is generated by chlormequat chloride and inorganic base in anhydrous organic solvent such as absolute ethyl alcohol, inorganic salt precipitate is filtered, and then the solution and lipoic acid are subjected to acid-base neutralization reaction, wherein the specific reaction formula is as follows:
ion exchange reaction: is prepared by ion exchange reaction of lipoic acid sodium salt and chlormequat chloride in solvent such as absolute ethyl alcohol. The specific reaction formula is as follows:
the high-temperature oxidation resistant ionic cotton topping agent provided by the invention can adopt three modes of manual spraying, mechanical spraying and unmanned aerial vehicle spraying, and the dosage of each hectare is 180 g.hm during manual spraying -2 The water consumption is 450kg hm -2 The method comprises the steps of carrying out a first treatment on the surface of the When the spraying agent is sprayed mechanically, the dosage per hectare is 210 g.hm -2 The water consumption is 600 kg/hm -2 The method comprises the steps of carrying out a first treatment on the surface of the The spraying application rate of the unmanned aerial vehicle is 150 g.hm -2 The water consumption is 8kg hm -2 The aerial photography of the application area and the application line before the application.
The cotton is sprayed once according to the instruction of use in the flowering phase (about 7 months and about 13 days), and the gibberellin activity in the plant body can be reduced through leaf absorption, so that the cell elongation is inhibited, the growth vigor of the terminal buds is weakened, the longitudinal and transverse growth of the plant is controlled, the internode of the plant is shortened, the plant type is compact, the leaf color is deep, the leaf area is reduced, the synthesis of chlorophyll is enhanced, the vigorous growth of the plant is prevented, the sealing is delayed and the like. The cotton boll is provided with enough nutrients, so that the cotton boll is enabled to be large and stable in fruit setting.
The optimal time for application is three days after cotton is watered, and the application is needed to be reapplied in case of rain within 8 hours after application before twelve am or after six pm on a sunny day.
Example 1
And (3) preparing the lipoic acid chlormequat chloride ionic liquid by adopting an acid-base neutralization reaction:
16.1g of 98% chlormequat chloride raw medicine (0.1 mol) and 5.6g of potassium hydroxide (0.1 mol) are dissolved in 80g of absolute ethyl alcohol, the mixture is added into a 250mL three-port bottle, the mixture is stirred and reacted at 25 ℃ until white crystal potassium chloride precipitate in a reaction system is not increased, the precipitate is filtered, 20.8g of 99% lipoic acid (0.1 mol) is added, stirring is carried out for 2 hours at room temperature, the reaction is stopped when the content of free chlormequat chloride in the detected solution is lower than 50mg/L, ethanol is removed by rotary evaporation, the lipoic acid chlormequat chloride ionic liquid is obtained, the yield is 98.5%, the viscosity is 112 centipoises, and the water aqua containing 47% of active ingredient chlormequat chloride mass fraction has the pH value of 7.2. The specific chemical reaction equation is as follows:
the chlormequat chloride solution containing 47% of chlormequat chloride serving as an active ingredient prepared in example 1 is used as a cotton topping agent for cotton topping, and the experimental effect is recorded: referring to (Wang Gang et al, china cotton, 2018) Xinjiang early-maturing upland cotton chemical topping technical protocol method design: the amount of the topping according to example 1 of the invention was 150 g.hm -2 Adding 8 kg/hm water -2 Spraying unmanned aerial vehicle, wherein the dosage of the topping agent of the comparative example 1 is 141g hm -2 Adding 8 kg/hm water -2 Spraying unmanned aerial vehicle, wherein the dosage of the topping agent of the comparative example 2 is 124g hm -2 Adding 8 kg/hm water -2 And spraying unmanned aerial vehicle. The preparation method is operated according to the requirements of GB/T8321.1-2000, and the preparation is used after being diluted for the second time, and the specific method comprises the following steps: firstly, 1 bucket and 1 measuring cup are prepared before dispensing, so as to ensure the accuracy of dispensing; and secondly, adding half of water into Shi Yaoxiang, pouring the dosage of the medicament required by weighing in a dosage cup into a water barrel to prepare mother liquor, adding the mother liquor into a medicament application box, simultaneously carrying out backwater stirring, and then filling water and stirring uniformly. The cotton topping agent with the mass fraction of 50% of chlormequat chloride water is selected as the cotton topping agent of the comparative example 1, the cotton topping agent with the mass fraction of 57% of chlormequat chloride water is selected as the comparative example 2, the cotton topping agent is selected as the comparative example 3 without using the cotton topping agent, the preparation method of the chlormequat chloride water is the same as that of the example 1, and the raw material proportion is adjusted according to the requirement that the mass fraction of chlormequat chloride is 57%.
The test floor is arranged in the newThe cultivation of ARA cotton is carried out in a 40 DEG 23'N,81 DEG 17' E region, 7d of topping treatment is carried out in a high temperature (day high temperature is more than or equal to 35 ℃) weather, and 7d of topping treatment is continued. The soil of the test field is loam, the previous stubble is cotton, and the organic matter content of the plough layer soil is 17.9g.kg -1 26.7mg.kg of alkaline hydrolysis nitrogen -1 Quick-acting phosphorus 24.6 mg.kg -1 Quick-acting potassium 188.0 mg.kg -1 . The cotton variety is Xinlun 75, which is covered by wide film, 1 film and 4 lines, the theoretical plant number is 21 ten thousand plants hm -2 The manual topping link is replaced by chemical topping and other modes are all according to the conventional management mode of the high-yield field.
To illustrate the effect of the present invention on cotton, the cotton topping agent of example 1, comparative example 2 and comparative example 3 of the present invention were tested in the ara reclamation area of Xinjiang, and the specific results thereof are shown in table 1.
TABLE 1 effects of different treatments of example 1, comparative example 2 and comparative example 3 on agronomic traits and yield of cotton
Note that: the above table data are all averages of three replicates per treatment, with different letters indicating significant differences at the level of P.ltoreq.0.05. The following is the same.
As can be seen from Table 1, compared with manual topping, the cotton topping agent of the invention omits the manual topping step, greatly reduces labor intensity and improves mechanical operation level, thereby reducing the cotton planting cost input per hectare by 780 yuan hms -2 The yield increase rate can reach 0.05%; compared with the treatment of comparative example 1 (chlormequat chloride single agent), the topping agent of the invention has the advantages that the average topping amount is increased by 1.1, the yield is increased by 14.3 percent, and the problem that the topping peach is easy to separate when the chlormequat chloride is singly used is avoided after the cotton topping agent of the invention is used; compared with the treatment of comparative example 2 (chlormequat salicylate), the topping agent of the invention has the advantages that the topping amount is increased by 0.8 on average, and the yield is increased by 4.8%. Taking Xinjiang (cotton planting area of 250 ten thousand hectares) as an example, compared with manual topping, the cotton topping agent of the invention can save the cost of 19.5 hundred million (780 yuan) of RMBX 250 kilohectares); compared with the treatment of comparative example 1, the yield per unit time is improved by 14.3 percent, and the yield-increasing RMB can reach 71.5 hundred million yuan (2 tons/hectare multiplied by 250 ten thousand hectares multiplied by 1 ten thousand yuan/ton multiplied by 14.3 percent); compared with the treatment of the comparative example 1, the unit yield is improved by 4.8 percent, and the income-increasing RMB can reach 24 hundred million yuan (2 tons/hectare multiplied by 250 hectares multiplied by 1 thousand yuan/ton multiplied by 4.8 percent). Therefore, the ionic topping agent provided by the invention has wide popularization value.
The extremely high temperature stress can aggravate the respiration of cotton, weaken photosynthesis and reduce pollen activity, so that a great amount of bolls fall off, and the yield and quality of the cotton in south Xinjiang are greatly affected. The physiological indexes of the stress resistance in the cotton body comprise superoxide dismutase SOD activity, peroxidase POD activity and malondialdehyde MDA content, and the physiological indexes of the stress resistance in the cotton body are affected by different degrees under high temperature stress. Superoxide dismutase SOD activity is measured by adopting a Nitrogen Blue Tetrazolium (NBT) method, peroxidase POD activity is measured by adopting a guaiacol method, and malondialdehyde MDA content is measured by adopting a thiobarbituric acid colorimetric method, so that data shown in figure 1 are obtained. Fig. 1 is a data comparison of SOD activity, POD activity and MDA content of cotton treated in example 1 (chlormequat lipoic acid prepared by acid-base neutralization), comparative example 1 (chlormequat salicylate), comparative example 2 (chlormequat salicylate), and comparative example 3 (artificial topping) under high temperature stress (weather of day high temperature not less than 35 ℃), in fig. 1, a is a data comparison of SOD activity, B is a data comparison of POD activity, and C is a data comparison of MDA content. As can be seen from fig. 1, when the temperature is stressed for 9 days, the SOD activity and POD activity of the cotton treated by the ionic topping agent provided by the invention are higher than those of the medicament control of comparative example 1 and the manual topping treatment of comparative example 3, and the MDA content is lower than that of the medicament control of comparative example 1 and the manual topping treatment of comparative example 2, so that the cotton shows better high temperature resistance.
Table 2 shows the results of example 1 (chlormequat lipoic acid), comparative example 1 (chlormequat chloride single agent), comparative example 2 (chlormequat salicylate) comparison of data of cotton quality of the cotton treated in comparative example 3 (artificial topping) after 7 days of high temperature stress (weather of day high temperature not less than 35 ℃). Table 2 shows that the breaking ratio strength of the cotton treated in example 1 of the present invention is significantly higher than that of the agent control of comparative example 1 and the artificial topping treatment of comparative example 3 after 7 days of high temperature stress, and the quality indexes of the rest cotton are not significantly different. The cotton topping agent treated cotton of example 1 of the present invention was shown to exhibit better tolerance when subjected to high temperature stress.
TABLE 2 effects of different treatments of example 1, comparative examples 1-3 on cotton quality
Example 2
The ion exchange reaction is adopted to prepare the lipoic acid chlormequat chloride ionic liquid:
16.1g of 98% chlormequat chloride raw material (0.1 mol) is dissolved by deionized water, 23.5g of 98% sodium lipoic acid (0.11 mol) is added, the reaction is stopped when the content of free chlormequat chloride in the solution is detected to be lower than 50mg/L after stirring for 2 hours at 40 ℃ to obtain an aqueous agent with the viscosity of 102 centipoises and 47% of the mass fraction of the chlormequat chloride as an active ingredient, and the pH value of the aqueous agent is 6.7. The specific chemical reaction equation is as follows:
the ionic liquid containing 47% of chlormequat chloride as an active ingredient prepared in example 2 was used as a cotton topping agent for cotton topping, and its experimental effect was recorded, and comparative analysis was performed with comparative example 1, comparative example 2 and comparative example 3, using the same method and amount as in example 1.
The test lands for comparative analysis of example 2 and comparative examples 1 to 3 were set in the cotton reclamation area (44 deg.65 'N,86 deg.43' E) of Xinjiang sand well, and 10d after topping was put into high temperature (daily high temperature: 35 ℃ C.) weather for 5d. The soil of the test field is loam, the previous stubble is cotton, and the organic matter content of the plough layer soil is 17.5 g.kg -1 25.0 mg/kg of alkaline hydrolysis nitrogen -1 22.5 mg/kg of quick-acting phosphorus -1 191.5 mg/kg of quick-acting potassium -1 . The cotton variety is Tahe No. 2, is covered by a wide film, and has 1 film and 4 lines, and the theoretical plant number is 21 ten thousand plants hm -2 Except that the manual topping ring joint is replaced by chemical topping, the process is carried out according to the conventional management mode of the high-yield field.
To illustrate the effect of the cotton of the present invention, the cotton topping agent of example 2 of the present invention, the conventional manual topping agent of comparative example 1, comparative example 2 and comparative example 3 were tested in parallel in the Xinjiang Sha Jingzi reclamation area, and the results are shown in Table 3.
TABLE 3 effects of different treatments of example 2, comparative example 1, comparative example 2 and comparative example 3 on cotton yield
As is clear from Table 3, the cotton topping treatment using the cotton topping agent of example 2 of the present invention reduced the cost input per hectare of cotton planting by 780 Yuan & hm -2 The yield increase rate can reach 0.06%; compared with the single-dose treatment of chlormequat chloride in comparative example 1, the topping agent in the embodiment 2 of the invention has the advantages that the average number of topping peaches is increased by 1.2, the yield is increased to 12.7%, and the problem that topping peaches are easy to separate when chlormequat chloride is singly used after the cotton topping agent in the embodiment 2 of the invention is used is avoided; compared with the treatment of comparative example 2 (chlormequat salicylate), the increase rate of the topping agent treatment of the invention reaches 2.5 percent. Taking Xinjiang (cotton planting area of 250 ten thousand hectares) as an example, the cotton topping agent of the embodiment 2 of the invention can save the cost of 19.5 hundred million yuan (780 yuan multiplied by 250 ten thousand hectares) of RMB compared with the manual topping of the comparative example 3; compared with the single-dose control medicament treatment of chlormequat chloride in comparative example 1, the single-dose control medicament treatment improves the unit yield by 12.86 percent, and the income-increasing RMB can reach 63.5 hundred million yuan (2 tons/hectare multiplied by 250 hectares multiplied by 1 ten thousand yuan/ton multiplied by 12.7 percent); compared with the treatment of the control medicament of chlormequat salicylate in comparative example 2, the single yield is improved by 2.5 percent, and the income-increasing RMB can reach 12.5 hundred million yuan (2 tons/hectare multiplied by 250 hectares multiplied by 1 thousand yuan/ton multiplied by 2.5 percent).
FIG. 2 shows the results of example 1 (chlormequat lipoic acid), comparative example 1 (chlormequat chloride single dose), comparative example 2 (chlormequat salicylate) data comparison of SOD activity, POD activity and MDA content of cotton treated by comparative example 3 (artificial topping) under high temperature stress (day high temperature is more than or equal to 35 ℃), in fig. 2, a is a comparison of SOD activity data, B is a comparison of POD activity data, and C is a comparison of MDA content data. As can be seen from fig. 2, when the cotton is stressed at high temperature for 9 days, the SOD activity and POD activity of the cotton treated in example 2 of the present invention are higher than those of the agent of comparative example 1, the agent of comparative example 2 and the artificial topping of comparative example 3, and the MDA content is lower than those of the agent of comparative example 1 and the artificial topping of comparative example 3, so that the cotton exhibits better high temperature resistance.
Table 4 shows the data comparison of cotton quality after 5 days of high temperature stress (day high temperature not less than 35 ℃ C.) for cotton treated in example 2 (chlormequat chloride lipoic acid prepared by ion exchange reaction), comparative example 1 (chlormequat chloride single dose), comparative example 2 (chlormequat salicylate), and comparative example 3 (artificial topping). Table 5 shows that the breaking strength of the cotton treated with the cotton topping agent of example 2 of the present invention is significantly higher than that of the agent control of comparative example 1 and the artificial topping treatment of comparative example 3 for 5 days under high temperature stress, and the remaining cotton quality indexes have no significant difference. The cotton topping agent treated cotton of example 2 of the present invention was shown to exhibit better tolerance when subjected to high temperature stress.
Table 4 effects of different treatments of example 2, comparative example 1, comparative example 2 and comparative example 3 on cotton quality
Example 3
And (3) preparing the lipoic acid chlormequat chloride ionic liquid by adopting an acid-base neutralization reaction:
16.1g of 98% chlormequat chloride raw medicine (0.1 mol) and 5.6g of potassium hydroxide (0.1 mol) are dissolved in 80g of absolute ethyl alcohol, the mixture is added into a 250mL three-port bottle, the mixture is stirred and reacted at 25 ℃ until white crystal potassium chloride precipitate in a reaction system is not increased, the precipitate is filtered, 20.8g of 99% lipoic acid (0.1 mol) is added, stirring is carried out for 2 hours at room temperature, the reaction is stopped when the content of free chlormequat chloride in the detected solution is lower than 50mg/L, ethanol is removed by rotary evaporation, the lipoic acid chlormequat chloride ionic liquid is obtained, the yield is 98.5%, the viscosity is 112 centipoises, and the water aqua containing 47% of active ingredient chlormequat chloride mass fraction has the pH value of 7.2. The specific chemical reaction equation is as follows:
the ionic liquid containing 47% of chlormequat chloride as an active ingredient prepared in example 3 was used as a cotton topping agent for cotton topping, and its experimental effect was recorded, and comparative analysis was performed with comparative example 1, comparative example 2 and comparative example 3, using the same method and amount as in example 1.
The experimental plots for comparative analyses of example 3, comparative example 1, comparative example 2 and comparative example 3 were set in Hami red Star City, xinjiang (42℃78'N,93℃43' E), and 5d after topping was put into high temperature (daily high temperature. Gtoreq.35℃) weather for 25d. The soil of the test field is sandy loam, the previous stubble is cotton, and the organic matter content of the plough layer soil is 16.5 g.kg -1 24.0 mg/kg of alkaline hydrolysis nitrogen -1 22 mg/kg of quick-acting phosphorus -1 Quick-acting potassium 193mg kg -1 . The cotton variety is Xinlun No. 67, which is covered by wide film, 1 film and 4 lines, the theoretical plant number is 21 ten thousand plants hm -2 Except that the manual topping ring joint is replaced by chemical topping, the process is carried out according to the conventional management mode of the high-yield field.
To illustrate the effect of the cotton of the present invention, the cotton topping agent of example 3 of the present invention, the conventional chemical topping of comparative example 1, and chlormequat chloride salicylate of comparative example 2, and the artificial topping of comparative example 3 were each tested in parallel in Hami red star city of Xinjiang, and the results are shown in Table 5.
TABLE 5 effects of different treatments of example 3, comparative example 1, comparative example 2 and comparative example 3 on cotton yield
As can be seen from Table 5, the cotton topping agent of example 3 of the present invention omits the manual topping step, greatly reduces labor intensity and improves the mechanical operation level, thereby reducing the cotton planting cost input per hectare by 780 yuan hm -2 Slightly reduced yield (-0.4%); compared with the single chlormequat chloride treatment in comparative example 1, the topping agent treatment of the invention of example 3 increases the average topping amount of the topping peaches by 0.5, and increases the yield by 9.3%, which shows that the topping agent treatment of the invention is usedAfter the cotton topping agent of example 3, the problem that the topping peach is easy to separate when chlormequat chloride is singly used is avoided. Taking Xinjiang (cotton planting area of 250 ten thousand hectares) as an example, the cotton topping agent of the embodiment 3 of the invention can save the cost of 19.5 hundred million yuan (780 yuan multiplied by 250 ten thousand hectares) of RMB compared with the manual topping of the comparative example 3; compared with the single-dose control medicament treatment of chlormequat chloride in comparative example 1, the single-dose control medicament treatment improves the single yield by 9.3 percent, and the income-increasing RMB can reach 46.5 hundred million yuan (2 tons/hectare multiplied by 250 hectares multiplied by 1 ten thousand yuan/ton multiplied by 9.3 percent), so the invention has wide popularization value.
Fig. 3 is a data comparison of SOD activity, POD activity and MDA content of cotton treated in example 3 (chlormequat lipoic acid prepared by acid-base neutralization), comparative example 1 (chlormequat salicylate), comparative example 2 (chlormequat salicylate), and comparative example 3 (artificial topping) under high temperature stress (weather of day high temperature not less than 35 ℃), wherein a is a data comparison of SOD activity, B is a data comparison of POD activity, and C is a data comparison of MDA content in fig. 3. As can be seen from fig. 3, the SOD activity and POD activity of the cotton treated in example 3 of the present invention are higher than those of the chemical controls of comparative example 1 and comparative example 2 and the artificial topping of comparative example 3, and the MDA content is lower than those of the chemical controls of comparative example 1 and comparative example 2 and the artificial topping of comparative example 3 at 9 days of high temperature stress, and the higher high temperature stress resistance is exhibited.
Table 6 shows that the cotton treated with the topping agent of the cotton of example 3 shows better oxidation resistance when subjected to high temperature stress, as shown in Table 6, after the cotton is subjected to high temperature stress (data comparison of cotton quality after 10 days in weather at a temperature of not less than 35 ℃ in daily high temperature), the cotton treated with the topping agent of the invention has significantly higher breaking specific strength than that of the cotton treated with comparative examples 1 to 3 in 10 days in high temperature.
TABLE 6 effects of different treatments of example 3, comparative examples 1-3 on cotton quality

Claims (13)

1. The ionic topping agent is characterized by comprising the following effective components in percentage by weight:
2. the ionic topping agent according to claim 1, wherein the raw materials for preparing the ionic topping agent comprise chlormequat chloride and lipoic acid.
3. The ionic topping agent according to claim 2, wherein the ionic topping agent is prepared by an acid-base neutralization reaction of chlormequat chloride and lipoic acid;
alternatively, the ionic topping agent is prepared by ion exchange reaction of chlormequat chloride and lipoate.
4. The ionic topping agent according to claim 3, wherein chlormequat chloride and inorganic base are placed in an anhydrous organic solvent for reaction, and inorganic salt precipitate is filtered to obtain chlormequat chloride quaternary ammonium alkaline solution.
5. The ionic capping agent of claim 4 wherein the inorganic base comprises one or more of potassium hydroxide, sodium hydroxide, barium hydroxide, calcium hydroxide, aluminum hydroxide, lithium hydroxide, or magnesium hydroxide.
6. The ionic capping agent of claim 4 wherein the inorganic base comprises potassium hydroxide.
7. The ionic capping agent of claim 3 or 4 wherein the lipoate salt comprises one or more of potassium lipoate, sodium lipoate, aluminum lipoate, magnesium lipoate.
8. The ionic topping agent according to claim 2, wherein the molar ratio of lipoic acid to chlormequat chloride is 1 (0.2-2).
9. The ionic topping agent according to claim 2, wherein the molar ratio of lipoic acid to chlormequat chloride is 1 (0.8-1).
10. The ionic topping agent according to claim 2, wherein the molar ratio of lipoic acid to chlormequat chloride is 1:1.
11. the ionic topping agent according to claim 3, wherein the acid-base neutralization reaction or the ion exchange reaction is carried out for 1 to 4 hours.
12. The ionic topping agent according to claim 3, wherein the acid-base neutralization reaction or the ion exchange reaction is carried out for 2 to 3 hours.
13. The use of an ionic topping according to any one of claims 1 to 12, wherein the ionic topping is a high temperature oxidation resistant ionic cotton topping.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108822077A (en) * 2018-08-07 2018-11-16 苏州富士莱医药股份有限公司 A kind of refining methd of r-lipoic acid cholinester halide
CN109180502A (en) * 2018-08-09 2019-01-11 绍兴东湖高科股份有限公司 Utilize the tubular reactor and method of cycocel production End gas production choline chloride
CN110476973A (en) * 2019-08-31 2019-11-22 中国农业科学院棉花研究所 A kind of cotton, which is planted, to be adjusted and its preparation and application
CN111206035A (en) * 2020-02-17 2020-05-29 河南科技学院 Gene and method for regulating senescence process of target plant leaves and application of gene and method to cotton crops
CN111567522A (en) * 2020-05-29 2020-08-25 高瑾 Cotton topping agent and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108822077A (en) * 2018-08-07 2018-11-16 苏州富士莱医药股份有限公司 A kind of refining methd of r-lipoic acid cholinester halide
CN109180502A (en) * 2018-08-09 2019-01-11 绍兴东湖高科股份有限公司 Utilize the tubular reactor and method of cycocel production End gas production choline chloride
CN110476973A (en) * 2019-08-31 2019-11-22 中国农业科学院棉花研究所 A kind of cotton, which is planted, to be adjusted and its preparation and application
CN111206035A (en) * 2020-02-17 2020-05-29 河南科技学院 Gene and method for regulating senescence process of target plant leaves and application of gene and method to cotton crops
CN111567522A (en) * 2020-05-29 2020-08-25 高瑾 Cotton topping agent and preparation method thereof

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