Carboxylated　cellulose　nanocrystals　(CNCs)　were　produced　from　cotton　linter　using　a　mixture　of　a　dicarboxylic　acid　(maleic　acid　or　succinic　acid)　and　its　corresponding　anhydride　with　or　without　catalyst　in　acetic　acid　as　solvent.　The　low　solubilities　of　these　dicarboxylic　acids　can　ease　chemical　recovery　and　decrease　environmental　impact　(especailly　maleic　acid　is　a　U.S.　FDA　approved　indirect　food　additive　(21CFR175-177))　and　capital　costs　compared　with　the　conventional　concentrated　sulfuric　acid　hydrolysis　for　producing　CNCs.　The　dicarboxylic-acid-produced　CNCs　(DC-CNCs)　contained　surface　carboxyl　groups　of　approximately　0.5　mmol/g,　with　ranges　of　dimensions　of　50–150　nm　in　diameter　and　50–700　nm　in　length.　Birefringence　was　observed　in　the　DC-CNC　suspensions　above　critical　concentrations.　However,　fingerprint　texture　was　only　observed　in　the　DC-CNC　suspensions　produced　with　catalyst　p-toluenesulfonic　acid.　Scanning　electron　microscopy　images　of　the　cross　section　of　DC-CNC　films　revealed　a　periodic　ordered　multilayer　structure.　DC-CNCs　were　also　produced　using　recycled　dicarboxylic　acids.　©　2021