CN1003302B - Composition of solide compound of ti-ascorbic acid used in auxin - Google Patents
Composition of solide compound of ti-ascorbic acid used in auxin Download PDFInfo
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- CN1003302B CN1003302B CN85107690.4A CN85107690A CN1003302B CN 1003302 B CN1003302 B CN 1003302B CN 85107690 A CN85107690 A CN 85107690A CN 1003302 B CN1003302 B CN 1003302B
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Abstract
The present invention relates to a synthetic method for a titanium-ascorbic acid solid compound of uncertain proportion, and the compound is used as plant growth regulators. Titanic salt solution and ascorbic acid solution are mixed according to a certain molar ratio, the final pH value of the solution is regulated to 5.0 to 10.8, and the titanium-ascorbic acid solid compound of uncertain proportion is generated. A mole ratio of the titanium to the ascorbic acid is 1:0.45 to 1.3, a preferable mole ratio is 1:0.5 to 0.7, and a preferable final pH value of the solution is 6 to 8. The synthetic method has the advantages of convenience and low cost. The compound has the advantages of stable property, no moisture absorption and easy long-term storage, can be used for regulating the growth of crops and fowls, and can increase yields of the crops and the fowls.
Description
The present invention relates to a kind of synthetic method of titanium-ascorbic acid solid chemical compound of indefinite composition, this solid chemical compound is soluble in water, can be used for regulating crop growth to increase its output and to improve its quality.
Titanium plays many-sided effect in plant growth and development process: promote the synthetic of photosynthesis and carbohydrate, increase the nitrogen fixing capacity that the root nodule number improves plant; Promote the absorption of plant to other trace element molybdenums, boron, iron, zinc, copper, manganese etc.But titanium ion very easily hydrolysis formation is difficult to by the precipitation of plant absorbing, and reduces its biologically active.
Some organic derivative that US3728365 and US3782917 have described with transition metals Ti, zirconium before the present invention reacts with the sulphur dioxide reaction or with the sulfonate reaction of hydrocarbon or with sulfinate, generate cyclopentadiene (IV-B organizes metal) hydrocarbon sulfonate or sulfinate, can be used as the volume increase agent of crops, and enumerated the example that titanic this compounds impels volume increase such as wheat, soybean.The storage of this class titanium solid compound and transport more convenient, but because to need to use the organic compound of metal in building-up process be raw material and a large amount of organic solvents; Also must be dissolved in the solvent during use or be dispersed in the dispersant, and cost is increased, influence its practical value.
Hungary HU3133/80 relates to the plant regulation promotor composition invention of a titanium.The plant regulation element of this titanium is a main component with titanium-ascorbic acid liquid-compound, the proportioning of titanic ion and ascorbic acid is 1 mole in this liquid-compound: the 14-28 mole adds one or more plant essential nutrients and one or more plant hormones, stabilizing agent and other adhesive agents and additive simultaneously.This liquid plant regulation element is sold as commodity production, and trade name is " TITAVIT ".For being suitable for using of crops, its pH value is transferred to 5-7.Because the amount ratio ti excess 50-100 of ascorbic acid doubly, and added stabilizing agent and other nutrients, adhesive agent etc., its stability is increased.Microorganism there is resistance, can reduces number of times, can keep being suitable for state in the time 2 years left and right sides to plant treatment, easy to use, the growths of crops there is good production-increasing function.But it is generally acknowledged when the amount of ascorbic acid is lower than the amount of titanium, even it also is unsettled generating the compound of titanium-ascorbic acid, in order to prevent the titanium ion hydrolytic precipitation, need heavy dose of expensive ascorbic acid that adopts, increased product cost, and because this plant regulation element is a liquid, packed and transported and storage are all inconvenient, and the cost of product is more increased.
British patent document GB2109217 report titanium tetrachloride and the faint yellow or rust solid titanium-ascorbic acid compound of solid ascorbic acid reaction generation are 1 mole through the mole ratio of conversion titanium and ascorbic acid: the 0.81-12.6 mole.But it is acid that this product is, and can't spray on crops.
First purpose of the present invention is synthetic a kind of stable in properties, can long preservation never degenerate, and titanium soluble in water-ascorbic acid solid chemical compound, can be used for regulating plant and growth of animals or poultry.Make it increase output.
Another object of the present invention is that a kind of technology of proposition is easy, the synthetic method of the titanium that cost is low-ascorbic acid solid chemical compound.
Titanium-ascorbic acid compound synthetic is to be raw material with titanium salt, ascorbic acid and alkali, and its synthetic method generally is that titanic solution is mixed according to a certain ratio with aqueous ascorbic acid, in order to make not hydrolysis of titanium, adds excessive ascorbic acid.According to the present invention, the titanium ion in the said tetravalent salt of titanium and the proportioning of ascorbic acid are 1 mole: the 0.45-0.77 mole, with the pH value of alkali regulator solution, making the final pH value is 5.0-8.0.The solid precipitation that generates is separated with solution, just obtained the titanium-ascorbic acid curing compound of indefinite composition.Because the final pH value is higher when synthetic, state such as titanium ion can dimerization, trimerization and ascorbic acid form solid chemical compound, therefore this compound is indefinite composition, the percetage by weight of its chemical analysis has a scope: titanium 12.7-24.8%, ascorbic acid 26-39%, ammonium ion 4.49-10.8%, chlorion 9.4-22.2%, following chemical components in percentage by weight is different because of synthesis condition and wash conditions.This compound is the rufous powder, and proportion 1.75-1.85 begins to decompose in the time of 70-80 ℃, this compound is soluble in water, and the pH value of its weak solution is 6.0-7.1, the solvability in water＞200 grams per liters, nonhygroscopic when solid-state, maximal increment is 1.5% under the condition of relative temperature 60-75%.The alkali of regulator solution pH value can be sodium hydroxide, potassium hydroxide and ammonium hydroxide, used raw material can be titanium tetrachlorides, the aqueous solution that titanium salts such as titanium sulfate and titanium potassium oxalate are made into, with chemical determination Ti concentration wherein, mix mutually with ascorbic acid solution in required ratio.
The compound method of aqueous ascorbic acid: a certain amount of ascorbic acid is water-soluble, fit over the aqueous ascorbic acid that concentration is 1 mol, the concentration of ascorbic acid stoste can change according to the concentration of titanium stoste, with in and the time be convenient to stir for good, stir difficulty when two kinds of original liquid concentrations are too high, cross rare reduction utilization rate of equipment and installations.
When synthetic, the proportioning of titanic ion and ascorbic acid is at 1 mole: in the 0.45-0.77 molar range, final pH value 5.0-8.0 could generate titanium soluble in water-ascorbic acid solid chemical compound.When the ascorbic acid of allocating in 1 mole of titanium ion was less than 0.45 mole, the poorly water-soluble of its product had the hydrolysate of titanium to produce.When proportioning is 1 mole: 0.45 mole, pH value＜5.0 o'clock do not have solid chemical compound generate.Various aqueous slkalis such as pH value available hydrogen potassium oxide, sodium hydroxide and the ammonium hydroxide of regulator solution.
When synthetic, the best proportioning of titanium salt and ascorbic acid is 1 mole: the 0.5-0.7 mole, the optimum range that forms the final pH value that titanium-ascorbic acid solid chemical compound of indefinite composition precipitates is 6-8.
For the bad sour solid chemical compound precipitation of the titanium-anti-blood that makes indefinite composition is separated better with solution, with titanium-ascorbic acid compound solid precipitation filtration, the drying of indefinite composition.
For this compound of purifying.The pH value of the most handy ammonium hydroxide regulator solution, and the titanium of this indefinite composition-ascorbic acid solid chemical compound precipitation is filtered easily, pH value with sodium hydroxide, potassium hydroxide regulator solution, the titanium of the indefinite composition that is generated-ascorbic acid solid chemical compound precipitation is difficult for filtering, and be difficult for purifying, can utilize the titanium-ascorbic acid curing compound of indefinite composition to be insoluble to ethanol, and the by-product ammonium chloride of reaction is dissolved in this * character of ethanol this compound of purifying.This compound can be used the ethanol rinsing in order to purify.Refilter drying.Titanium-ascorbic acid the solid chemical compound of the indefinite composition after purifying is easy to oven dry and grinds.The pH value that has now found that the titanium-ascorbic acid solid chemical compound precipitation that generates this indefinite composition is relevant with the proportioning of titanium and ascorbic acid, along with increasing of ascorbic acid amount in titanium and the ascorbic acid proportioning, the pH value that begins to occur the titanium-ascorbic acid solid chemical compound precipitation of indefinite composition also increases, and can adopt higher final pH value in this case; When the amount of allocating ascorbic acid into reduced, the pH value that begins to occur the titanium-ascorbic acid curing compound precipitation of indefinite composition also just reduced, and can adopt lower final pH value under the situation of here.
Under the situation of same proportioning, the final pH value is got when hanging down, the titanium of indefinite composition-ascorbic acid solid chemical compound good water solubility, but productive rate is low, and the final pH value increases, and productive rate increases, and the product water dissolubility reduces.Under same final pH value condition, along with the increase of the ascorbic acid amount in titanium and the ascorbic acid proportioning, the titanium of indefinite composition-ascorbic acid solid chemical compound productive rate reduces.The proportioning of titanium ion and ascorbic acid is 1 mole in the titanium salt: the 0.5-0.7 mole, titanium-ascorbic acid the solid chemical compound of the indefinite composition of gained has good water-solubility under the optimum condition when final pH scope that precipitates the titanium-ascorbic acid solid chemical compound of indefinite composition is 6-8, and the productive rate height, cost is low.Productive rate is lower when the final pH of the titanium-ascorbic acid solid chemical compound that precipitates indefinite composition is 5.0-6.0, and the amount of the ascorbic acid that pH＞8 o'clock are allocated into will increase, the consumption of ammonium hydroxide in a disguised form should increase when regulating pH, has increased consumption of raw materials, and product cost is increased.
The titanium of resulting indefinite composition-ascorbic acid solid chemical compound is dried in thermostatic drying chamber after filtering.
Differential thermal analysis curve according to the titanium-ascorbic acid solid chemical compound of indefinite composition is learnt, this curing compound begins to decompose in the time of 70-80 ℃, so the Controllable Temperature of oven dry is built in room temperature to 70 ℃, preferably be controlled between 40-70 ℃, time in oven dry below 40 ℃ is longer, the porcelain alms bowl grind into powder of the solid chemical compound after the drying.
The titanium of figure one, indefinite composition-ascorbic acid solid chemical compound differential thermal analysis curve.
The preparation condition of sample: titanium: ascorbic acid=1 mole: 0.65 mole, final pH=7, titaniferous 21.7% in the product.
Sample is heavy: 83.5 milligrams, and the check weighing range: 100 milligrams, temperature range: 10mv, differential thermal range: ± 25 μ V.
Abscissa is time (t) among the figure, with a minute expression.Ordinate is: T: temperature, curve T is a heating curve among the figure, curve from top to bottom, maximum temperature rises to 600 ℃.DTA: differential thermal curve, peak point are the endothermic reaction downwards, upwards are exothermic reaction; TG: thermogravimetric curve, example weight over time, curve from low to high, weight alleviates gradually.
Figure two, ascorbic acid infrared spectrogram
Tester: PERKIN-ELMER180
Abscissa is wave number cm, and ordinate is an extinction, 0.0-1.5.
Method for making sample: pressing potassium bromide troche, energy mode: const I
0, gain 1; Retouch flyback time: good 10, coarse 1, suppress 6, slit programme 6, time constant 6; Parameter mode: C.
The titanium of figure three, indefinite composition-ascorbic acid solid chemical compound infrared spectrogram
Sample preparation condition: proportioning: titanium: ascorbic acid=1 mole: 0.65 mole, final pH=7, washing with alcohol 3 times.
Abscissa is wave number cm, ordinate is an extinction, 0.0-1.5, compare the infrared spectrogram of ascorbic acid and indefinite composition titanium-ascorbic acid solid chemical compound, the OH peak in the infrared spectrogram of the titanium of indefinite composition-ascorbic acid solid chemical compound has obviously played variation as can be seen, and the absworption peak of its C=0 key is intact, displacement has only taken place, the sign that the C=0 key is not opened is described, but the absworption peak of its fingerprint region tails off, chemical combination has taken place according to salify theoretical explanation titanic and ascorbic acid.
Advantage of the present invention is: the first, and the synthetic method of the titanium of indefinite composition-ascorbic acid solid chemical compound is simple, and the consumption owing to ascorbic acid in synthetic significantly reduces, thereby has reduced the cost of product.The raw material that titanium-the ascorbic acid solid chemical compound is consumed of producing the indefinite composition of titaniferous 1 gram needs smart titanium tetrachloride 4.21 grams, ascorbic acid 2.53 grams, ammonium hydroxide (liquid specific gravity is 0.902) 7.9 grams, and during the titanium-ascorbic acid of synthetic every liter of titaniferous 1 gram of the method for Hungary HU3133/80-compound, titanium: the ascorbic acid weight ratio is 1: 100, the smart titanium tetrachloride of the raw material that consumed is 4.0 grams, ascorbic acid 100 grams, potassium hydroxide 33 grams.
The second, the titanium-ascorbic acid solid chemical compound of the indefinite composition of producing with synthetic method of the present invention is the rufous powder, and stable in properties is nonhygroscopic, can long preservation, and packed and transported is convenient, and is soluble in water, and hydrolytic precipitation does not take place, easy to use.The titanium of indefinite composition of the present invention-ascorbic acid solid chemical compound can be used for regulating the growth of crops and livestock and poultry, makes it increase output, behind for example potted plant rape this product solution through spraying 2.5ppm, can increase production 16%.
Three, the titanium of indefinite composition of the present invention-ascorbic acid solid chemical compound can mix use with various trace elements such as boron, iron, zinc, manganese, copper, molybdenums according to different situations and needs, improves plant to various trace elements absorbed.
Four, the titanium of indefinite composition of the present invention-ascorbic acid solid chemical compound is applicable to natural water, distilled water, and ion exchange water, to desired concn, the solution for preparing can be used for seed dressing towards rare in dissolving, soaks seed and sprays etc.
Five, the titanium of indefinite composition of the present invention-ascorbic acid solid chemical compound can with auximone commonly used, wetting agent and weed killer herbicide etc. mix to use.
Following example is just in order to further specify the present invention, rather than as the restriction of the scope of the invention, protection scope of the present invention is determined by claims.
Example 1
The proportioning of titanium and ascorbic acid is 1 mole: 0.5 mole, 176.12 gram content are no less than 99.7% ascorbic acid (BJ Pharmaceutical Co., Ltd.) to be dissolved in 1 premium on currency, (smeltery, Fushun produces will not have crystal's titanium tetrachloride again, contain Ti25%, proportion 1.727) 221.9 milliliters, under stirring condition, slowly be added in the aqueous ascorbic acid, drip the pH value of industrial hydrogen amine-oxides regulator solution after waiting to stir, make the titanium-ascorbic acid solid chemical compound precipitation that indefinite composition occurs, it is 5 that continuation adding ammonium hydroxide makes the final pH value of solution, this synthetic reaction is at room temperature carried out, but because the neutralization reaction heat release rises between 35-50 ℃ temperature of reaction system, this temperature with in relevant with speed.Titanium-ascorbic acid solid chemical compound the sedimentation and filtration of indefinite composition is drained, for the titanium of purifying-ascorbic acid solid chemical compound, filter cake can be used ethanol rinsing 1-2 time, levigate through under 60-70 ℃ of temperature, drying after the vacuum filtration again, the percentage by weight of the titanium of the indefinite composition after the purification-ascorbic acid solid chemical compound chemical composition is: titanium 24.2%, ascorbic acid 39%, ammonium ion 5.21%, chlorine 9.4%, a yield of titanium is 90.48%.
Example 2
Synthetic method is with example 1, only the proportioning of titanium and ascorbic acid is 1 mole: 0.45 mole, the ascorbic acid amount is 176.12 grams, no crystal's titanium tetrachloride amount is 246.5% milliliter, final pH is 5, and the yield of Ti is 90.26%, and the percentage by weight of the titanium of the indefinite composition after the purification-ascorbic acid solid chemical compound chemical composition is: titanium 24.8%, ascorbic acid 33%, ammonium ion 5.50%.40 °-60 ℃ of bake out temperatures.
Example 3
Synthetic method is with example 1, only the proportioning of titanium and ascorbic acid is 1 mole: 0.55 mole, the ascorbic acid amount is 176.12 grams, no crystal's titanium tetrachloride amount is 201.7% milliliter, and final pH is 8, and the yield of Ti is 93.58%, the percentage by weight of the titanium after the purification-ascorbic acid solid chemical compound chemical composition is respectively: titanium 22.4%, ascorbic acid 30%, ammonium ion 6.62%, chlorine 10.5%.
Example 4
Synthetic method is with example 1, only the proportioning of titanium and ascorbic acid is 1 mole: 0.65 mole, the ascorbic acid amount is 176.12 grams, no crystal's titanium tetrachloride amount is 170.7% milliliter, and final pH is 6, and the yield of Ti is 75.10%, the percetage by weight of the titanium after the purification-ascorbic acid solid chemical compound chemical composition is respectively: titanium 22.10%, ascorbic acid 38%, ammonium ion 5.12%, chlorion 11.70%.
Example 5
Synthetic method is with example 1, only the proportioning of titanium and ascorbic acid is 1 mole: 0.71 mole, ascorbic acid is 176.12 grams, no crystal's titanium tetrachloride amount is 156.3% milliliter, and final pH is 8, and the yield of Ti is 84.89%, the percetage by weight of the titanium after the purification-ascorbic acid solid chemical compound chemical composition is respectively: titanium 20.7%, ascorbic acid 30%, ammonium ion 5.85%, chlorion 11.2%.
Example 6
Synthetic method is with example 1, only the proportioning of titanium and ascorbic acid is 1 mole: 0.77 mole, the ascorbic acid amount is 176.12 grams, no crystal's titanium tetrachloride amount is 144.1 milliliters, and final pH is 7, and the yield of Ti is 57%, the percetage by weight of the titanium after the purification-ascorbic acid solid chemical compound chemical composition is respectively: titanium 20.7%, ascorbic acid 26%, ammonium ion 7.74%, chlorion 11.6%.
Example 7
Synthetic method is with example 1, and only the proportioning of titanium and ascorbic acid is 1 mole: 0.65 mole, as synthesis material, the final pH value of precipitation is 6 with titanium sulfate solution, and product titaniferous amount is 12.7%, is difficult for purifying, and the yield of Ti is 80.9%.
Example 8
Synthetic method is with example 1, only the proportioning of titanium and ascorbic acid is 1 mole: 0.65 mole, the ascorbic acid amount is 176.12 grams, no crystal's titanium tetrachloride amount is 170.7 milliliters, and final pH is 7, and the yield of Ti is 81.8%, percetage by weight without the titanium-ascorbic acid solid chemical compound chemical composition after purifying is respectively: titanium 17.4%, ascorbic acid 29%, ammonium ion 10.8%, chlorion 22.2%.
Be made into after weak solution sprays crops (cereal crops, vegetables, fruit etc.) with the titanium-ascorbic acid solid chemical compound of indefinite composition, growth or the volume increase of crop all produced effect.
Example A
Titanium-ascorbic acid the solid chemical compound of the indefinite composition that makes with said method is made into weak solution corn is carried out seedling growth test, and seed soaks the back germination through the titaniferous solution of variable concentrations, and the situation of emerging is as follows:
Wherein remarkable to the influence of corn growing way in seedling stage with the solution of titaniferous 3ppm, average plant height comparison is according to increasing by 15.9%, and average root length increases by 16%, and average leaf heavily increases by 33.9%.
Can use deionized water, distilled water when preparing weak solution with the titanium-ascorbic acid solid chemical compound of indefinite composition, also available natural water, running water, but because the composition more complicated in the natural water of various places, except that the pH value changed, calcium, the isoionic content range of magnesium fluctuateed bigger, and therefore the weak solution that is made into should not be put for a long time, preferably with using with joining, if put for a long time can add some citric acids or potassium citrate when precipitation occurring in right amount, sodium makes its dissolving.
Example B
Titanium-ascorbic acid the solid chemical compound of the indefinite composition that makes with said method is made into titaniferous 5ppm weak solution and sprays little rape, and following result is the mean value of four repeated tests:
Example C
The weak solution that the titanium-ascorbic acid solid chemical compound of the indefinite composition that makes with said method is made into titaniferous 2ppm sprays eggplant, and following result is four mean values that repeat.
Example D
The solution that the titanium-ascorbic acid solid chemical compound of the indefinite composition that makes with said method is made into titaniferous 5ppm sprays tomato, sprays at the tomato initial bloom stage for the first time, carries out after five weeks spraying second time, and following result is the mean values of four repetitions
Example E
The aqueous solution that the titanium-ascorbic acid solid chemical compound of the indefinite composition that makes with said method is made into titaniferous 10ppm sprays summer radish, sprays after plant enters the root expanding stage.After once spraying, no matter be that single-strain fresh weight or every basin fresh weight all show volume increase in various degree.
Example F
The indefinite composition titanium-ascorbic acid solid chemical compound that makes with said method is dissolved in water, be made into the solution of titaniferous 5ppm, two kinds of strawberries " Beijing heart " and " precious hand over early give birth to " are carried out three times spray, result of the test shows that strawberry output improves, and Vitamin C content increases.
In addition, the titanium of indefinite composition-ascorbic acid solid chemical compound can be used as feed addictive and carries out animal feeding, promotes growth of animal.Be used for feeding chicken, add 0.1% additive in the per kilogram feed, the daily gain of chicken can improve about 5%; Be used to feed pigs, the per kilogram feed adds 450 milligrams of these compounds, and the daily gain of pig can improve 4-13%.
Table A
The average plant height of the concentration of titanium (centimetre) average root length (centimetre) average leaf heavy (gram)
The 0(contrast) 27.4 24.4 0.56
1ppm 30.4 28.4 0.64
3ppm 32.1 28.3 0.75
5ppm 28.2 27.9 0.73
10ppm 28.7 25.8 0.73
30ppm 25.6 23.8 0.62
Table B
Output (gram/basin) productive rate (%)
Contrast 258 100
Spray behind the titanium 325 126
Table C
Output (jin/sub-district) productive rate (%)
Contrast 5.4 100
Spray behind the titanium 6.8 125
Table D
Output (jin/sub-district) productive rate (%)
Contrast 32.4 100
Spray behind the titanium 35.7 117
Table E
Production and productivity
(gram/basin) (gram/strain) (%)
Contrast 17.8 5.9 100
Spray behind the titanium 26.3 8.8 149
Table F
Amount to per mu yield (jin)
Strawberry cultivars volume increase (%)
Behind the contrast spray titanium
Beijing heart 142.8 170.9 19.6
The precious friendship early gives birth to 97.2 122.8 26.4
Claims (6)
1, the synthetic method of titanium-ascorbic acid compound of using of a plant growth regulators is with tetravalent salt of titanium solution and ascorbic acid aqueous solution, pH value with the alkali regulator solution, feature of the present invention is: the titanium ion in the said tetravalent salt of titanium and the proportioning of ascorbic acid are 1 mole: the 0.45-0.77 mole, said pH value finally is adjusted to 5.0-8.0, and titanium-ascorbic acid solid chemical compound precipitation of the indefinite composition that generates is separated with solution.
2, according to the synthetic method of a kind of titanium-ascorbic acid compound of claim 1, it is characterized in that the proportioning of titanium ion and ascorbic acid is 1 mole of 0.5-0.7 mole in the said tetravalent salt of titanium.
3,, it is characterized in that the final pH value of titanium-ascorbic acid curing compound precipitation of formed indefinite composition is 6-8 according to the synthetic method of a kind of titanium-ascorbic acid compound of claim 1.
4, according to the synthetic method of a kind of titanium-ascorbic acid compound of claim 1, it is characterized in that said alkali is ammonium hydroxide.
5, according to the synthetic method of claim 2,3, a kind of titanium-ascorbic acid compound of 4, it is characterized in that, with the titanium-ascorbic acid curing compound purifying of ethanol with said indefinite composition.
6, according to the synthetic method of a kind of titanium-ascorbic acid compound of claim 5, it is characterized in that, the titanium-ascorbic acid curing compound of indefinite composition is deposited under 40 ° to 70 ℃ the temperature and dries.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85107690.4A CN1003302B (en) | 1985-10-22 | 1985-10-22 | Composition of solide compound of ti-ascorbic acid used in auxin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85107690.4A CN1003302B (en) | 1985-10-22 | 1985-10-22 | Composition of solide compound of ti-ascorbic acid used in auxin |
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| CN1003302B true CN1003302B (en) | 1989-02-15 |
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| CN101665385B (en) * | 2009-09-16 | 2012-10-31 | 钛谷（天津）科技有限公司 | Process and device for producing hydrolytic stabilizing iron titanium by continuation method |
| CN104774142B (en) * | 2015-01-09 | 2017-08-25 | 河北科技师范学院 | A kind of no-solvent process for preparing solid organic acid titanium |
| PL239086B1 (en) | 2017-05-15 | 2021-11-02 | Intermag Spolka Z Ograniczona Odpowiedzialnoscia | Complexes of metal and ascorbic acid, method for obtaining them and applications |
| CN113519524A (en) * | 2020-04-21 | 2021-10-22 | 黄荣茂 | Plant immunomodulator and application thereof |
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