Glyoxylic acid (English glyoxylicacid), also known as formylformic acid, hydrated glyoxylic acid, and oxoacetic acid, has the chemical formula C2H203. It is the most basic aldehyde acid and is located in immature fruits, young environment-friendly leaves, and sugar beets. Those taken shape from water are monoclinic crystals (having 1/2 crystal water). Relative molecular mass 70.04. Melting point 98 ℃. It has an undesirable odor and is a highly harsh acid that is conveniently deliquescent and can develop a slurry when revealed to the air. Somewhat soluble in ethanol, ether and benzene, and soluble in water. The liquid option is very stable airborne and does not weaken. Exists in hydrated type in liquid solution. Reacts with a lot of steels except stainless steel. It has both acid and aldehyde residential or commercial properties. It can include with sodium bisulfite or hydrocyanic acid, react with hydroxylamine or phenylhydrazine to form oxime or hydrazone, can undertake silver mirror reaction, can happen in Canizzaro response, and can also generate carboxylates and esters, and so on.
Glyoxylic Acid Property
1.33 g/mL at 20 °C
14hPa at 19.85℃
Store below +30°C.
Miscible with ethanol. Slightly miscible with ether and benzene. Immiscible with esters.
Colorless to Light orange to Yellow
Glyoxylic Acid Uses
Glyoxylic acid is a fundamental organic chemical resources. It can be utilized to make the scent of cosmetics, everyday chemicals and food.
Used clinically as a good healing agent for skin wounds.
Biologically, plant development regulatory authorities, etc. Non-ferrous steel electroplating uses glyoxylic acid as the lowering agent as opposed to harmful chemicals (such as formaldehyde). In commercial pure light weight aluminum wafers, commercial pure titanium wafers, silicon wafers with TiN as the diffusion protective layer and silicon wafers with TiSiN as the diffusion protective layer Electroless copper plating has been attained for difficult-to-plat products such as copper plating. The evaluation results of the surface area morphology and grain framework of the coated copper plating layer reveal that different substratums have an excellent impact on the business structure of the copper plating layer, particularly in silicon wafers with TiN as the diffusion protective layer. And on the silicon wafer with TiSiN as the diffusion protective layer, a more precise particle composed of fragments with a typical size of 50 nm was acquired.
Synthesis of Glyoxylic Acid in Microchannel Reactor
The experimental device is received Figure 1. Nitric acid and glyoxal are pumped right into the microreactor via pump 1 and pump 2 respectively according to a molar proportion of 0.85:1. The experiment is executed utilizing segmented temperature control. At the t1 temperature, glyoxal and glyoxal are The nitric acid is combined and responded in the activator, and the combined solution continues to respond in the microchannel at t2 temperature level; after that the response is satiated in an area of coil linked to the microchannel at 10 to 15 ° C, and the reaction service enters the collection container via the back pressure shutoff, the product is gotten for evaluation.
When the molar proportion of nitric acid (35%) to glyoxal (40%) is 0.85:1, the glyoxal flow price (Q1) is 4.7 mL/min and the nitric acid circulation price (Q2) is 5.3 mL/min. The total house time is 4min54s, of which the home time in section t1 is 54s and the home time in area t2 is 4min. When the back pressure valve pressure is 0.5 MPa, the impact of temperature on conversion price and selectivity is as shown in the table. Figure 2 shows keeping the t2 temperature level at 40 ° C and analyzing the influencing factors of the t1 temperature. Figure 3 shows controlling the t1 temperature level to 80 ° C and analyzing the influencing variables of the t2 temperature level.
It can be ended from Figure 2 and Number 3 that when t1 raises from 40 ° C to 90 ° C, the conversion rate increases from 15% to 95%, the selectivity boosts from 20% to 58%, and after that lowers to 45%. The factor might be that when the temperature level is lower, the response price is slower and only a small amount of glyoxal is oxidized by nitric acid. As the temperature level increases, the response is gradually launched, so the conversion price and selectivity rise; but when the temperature is raised from 80 As the temperature continues to rise, the item will certainly remain to be oxidized right into oxalic acid, so the selectivity reduces; when t1 = 40 ° C, the temperature is reduced, and it is harder for glyoxal to be oxidized, and glyoxal is easy to polymerize and develop More autopolymers and consequently lower selectivity. When t2 increases from 20 ° C to 50 ° C, the conversion rate increases from 70% to 90%, and the selectivity boosts from 42% to 60%, and afterwards lowers to 40%. Analysis of the reason may be that the reaction has been started at the t1 temperature level. At the t2 temperature, glyoxal continues to join the reaction, so the conversion rate boosts; when t2 boosts from 20 ° C to 40 ° C, due to the polymerized glyoxal After preheating for an amount of time at the t1 temperature level, the existing component begins to depolymerize. At the t2 temperature, although the temperature level is reduced, the depolymerization reaction can not quit right away. Currently, the depolymerization rate is above the polymerization price, so the selectivity slowly raises. When t2 remains to increase from 40 ° C, the conversion of glyoxylic acid to oxalic acid is advertised, so the selectivity decreases. As a result, t1 = 80 ° C and t2 = 40 ° C were chosen in the next experiment.
NO is produced throughout the oxidation of glyoxal by nitric acid. Researches have actually shown that the visibility of NO in the system advertises the oxidation of glyoxal, that is, NO reacts with nitric acid to generate nitrous acid, and afterwards nitrous acid reacts with glyoxal to create Glyoxylic acid. Under the conditions of gas promo, pressure likewise plays a terrific duty in promoting the reaction. Number 4 reveals the effect of stress on the conversion price and selectivity of the response. This figure reveals that when the pressure increases, the conversion rate and selectivity of the reaction increase. This is due to the fact that when the pressure is low, the mixing effect in the system is poor and the system is unstable. Nonetheless, when the stress continues to boost, it is challenging to separate the NO created from glyoxylic acid. When glyoxylic acid and nitric acid are called and mixed, the nitrous acid created straight responds with glyoxylic acid, creating the nitrous acid in contact with glyoxal in the system to The content reduces and the response price reductions, so the conversion price and selectivity decline at the same time. As a result, the pressure of 1.0 MPa is the very best choice during the response procedure.
The trouble of this procedure is to stop the peroxidation of glyoxal. Therefore, in addition to the influencing elements that have to be considered in traditional reactors such as temperature and stress, staged feeding can additionally be taken into consideration. If the first feed quantity is also small, the reaction rate will certainly be reduced and the response time will be lengthened; if the initial feed quantity is way too much, glyoxylic acid will certainly be easily oxidized, which will quickly lead to a decrease in selectivity. In the process of making use of a microchannel reactor to accomplish connection, very first feed the initial response item with a molar proportion of nitric acid to glyoxal from 0.3:1, and after that include 0.12 mol of nitric acid to the 3rd reaction piece. This way, the conversion rate and selectivity of the reaction can reach more than 70%. Additionally, compared with the standard pot procedure, the quantity of nitric acid utilized in the whole response process is lowered, and the post-processing pressure is reduced.
This type of nitric acid oxidation reaction releases a lot of heat, and peroxidation products are conveniently produced during the reaction. Since the microchannel reactor has excellent heat transfer and warm transfer effects, it can accurately manage the reaction problems. For that reason, for response types where the temperature level is difficult to regulate in standard activators or where the selectivity of the response is reduced due to backmixing, better speculative outcomes can be accomplished through segmented temperature control and segmented feeding in microchannel reactors. Compared to typical pot responses, the advantages of microchannel activators are mainly reflected in:
① Experimental control of reaction problems (temperature, stress, flow) accurately.
② Double-sided warm exchange has excellent advantages for chain reactions with large heat dissipation.
③ Continual flow activator, without back-mixing, raises the selectivity of the response.
④ It inhabits a small location and can be used in chemical plant and research laboratory experiments.
Glyoxylic Acid Preparation Method
Presently, glyoxylic acid is mostly generated by glyoxal nitric acid oxidation approach in industry. Glyoxylic acid commercial products are usually 40% or 50% glyoxylic acid liquid option, which contains 0.7% -1.5% oxalic acid, 0.5% -1.5% glyoxal and 0.1% -3% hydrochloric acid contaminations. The glyoxal contamination in glyoxylic acid has an excellent influence on its top quality, and a lot of research has been carried out to minimize the content of glyoxal impurities in the product. In order to reduce the glyoxal residue in glyoxylic acid items in commercial production, the technique of including too much nitric acid to improve the conversion price of glyoxal basic materials has to be embraced, which causes the oxidative disintegration of a large amount of glyoxylic acid and decreases the item yield.
A method for preparing crystalline glyoxylic acid, which is defined because taking shape and preparing high-purity crystalline glyoxylic acid from a 45% -50% glyoxylic acid liquid option consists of the following steps:
( 1) Concentrate 35% -40% glyoxylic acid crude product under vacuum at 45-55 ° C to get 45% -50% glyoxylic acid; ( 2) Amazing 45% -50% glyoxylic acid to -2 -2 ° C, and centrifuge to divide the precipitated oxalic acid; ( 3) The mom liquor is more cooled down to -6 -10 ° C, and glyoxylic acid seed crystals are utilized to induce condensation of glyoxylic acid monohydrate;
( 4) Glyoxylic acid monohydrate crystals divided by centrifugation after 4-6 hours of low-temperature crystallization; ( 5) Repeat the above concentration and condensation splitting up operations of glyoxylic acid monohydrate for the second mommy alcohol; ( 6) 3 times the mother alcohol is returned to oxidation to decrease the glyoxal content and after that flowed; ( 7) Place the glyoxylic acid monohydrate crystals into a desiccator including anhydrous calcium chloride and calcium oxide to dry.
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ZhiShang Chemical is owned by ZhiShang Group is a professional new-type chemicals enterprise combined into research and development, production and sales .
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